1_Experiment 2-Purification of Sodium Chloride

Experiment 2: Purification of Sodium Chloride
[Experimental Objectives]
1. Master the knowledge of salt solubility and its application in inorganic
purification.
2. Learn to chemically purify the crude table salt and provide raw materials for
further refining of reagent grade of sodium chloride.
3. Learn the basic operations of solution, filtration, evaporation, crystallization,
vacuum filtration, the use of pH test paper, drying inorganic salt and so on.
[Fundamental Principles]
Sodium chloride with higher purity is prepared by purification of crude table
salt. Crude table salt contains not only insoluble impurities such as sediment, but
also soluble impurities such as Ca2+, Mg2+, K+, SO42- and so on. Insoluble impurities
can be removed by filtration. It is difficult to purify sodium chloride by
recrystallization because its solubility varies little with temperature. Ion separation
is needed by chemical method. Soluble impurities such as Ca 2+, Mg2+, SO42- can be
removed by selecting suitable reagents to form insoluble compounds. The procedure
is: Firstly, add excess BaCl2 solution to the crude table salt solution, so that SO42- is
converted to BaSO4 precipitation.
Ba2+ + SO42－ → BaSO4↓
Filter the precipitation and add excess NaOH and Na2CO3 solution to the filtrate
to precipitate Ca2+, Mg2+ and the remaining Ba2+ together.
Ca2+ + CO32－ → CaCO3↓
2Mg2+ + CO32－+2OH－ → Mg(OH)2∙ MgCO3↓
Ba2+ + CO32－ → BaCO3↓
Filter the precipitation again and neutralize the NaOH and Na 2CO3 remaining
in the filtrate with dilute HCl solution:
H+ +OH－ → H2O
2H+ + CO32－ → CO2 ↑+ H2O
K+ in crude table salt does not work with the above reagents, and remains in the
solution. Because the solubility of KCl is higher than that of NaCl when being heated,
and the content of KCl in crude table salt is very small, NaCl crystallizes and
precipitates during evaporation and concentration, and KCl remains in mother
solution to achieve separation. A small amount of excess hydrochloric acid escapes
in the form of hydrogen chloride when drying NaCl so as to purify NaCl.
[Apparatus, Medicine and Other Materials]

Platform scale, beaker (100 mL×2), graduated cylinder (10 mL, 50 mL), glass
funnel, funnel holder, Buchner funnel (φ5cm), suction filter bottle (250 mL),
porcelain casserole, test tube, dropper, drip plate, electric hot plate, vacuum pump
and the decompression system.
HCl (2 mol/L), NaOH (2 mol/L), BaCl2 (1 mol/L), Na2CO3 (1 mol/L),
(NH4)2C2O4 (0.5 mol/L), Magnesium reagent (dissolve 0.01g magnesium reagent
into the NaOH solution of 2 mol/L)
Crude table salt (s), pH test paper, filter paper.
[Experimental Procedures]
1. Purification of the crude table salt
(1) Weigh 8.0 g of crude table salt on a platform scale and put it in a beaker of
100 mL. Then add 30 mL of distilled water and dissolve it by heating and stirring.
When the solution is near boiling, drip BaCl2 solution of 1 mol/L drop by drop until
SO42- is completely generates white precipitation (about consuming 2 mL of BaCl 2
solution). In order to check whether the SO42- have precipitated completely, move
the beaker to the table to rest for a moment. After sedimentation, add 1-2 drops of
BaCl2 solution along the wall of the beaker, and observe whether there is turbidity
in the supernatant solution. If there was no turbidity, SO42- precipitate completely. If
it was turbid, continue to drip BaCl2 solution until they precipitate completely.
Continue to heat for 2~3 minutes, so that the precipitated particles grow bigger. After
cooling, use glass funnel to filter into another beaker, and discard the precipitation.
(2) Add 1mL of NaOH solution of 2 mol/L and 3mL of Na2CO3 solution of 1
mol/L to the filtrate and heat it to boiling. Check whether they have precipitated
completely with Na2CO3 solution. When the precipitation is complete, continue to
heat for 2-3 minutes. Filter the filtrate into the porcelain casserole by glass funnel
and discard the precipitation.
(3) Add HCl solution of 2 mol/L to the filtrate drop by drop and stir it
thoroughly. Check the pH value of the solution, until the pH value of the filtrate is
about 4. Evaporate and concentrate it to paste liquid on the electric heating plate.
(when the NaCl crystal film appears, keep stirring, but do not evaporate to dryness!)
Move it into the Brinell funnel before cooling and drain the remaining mother
solution.
(4) Move the crystal into the porcelain casserole and dry it slowly on the electric
heating plate (keep stirring to avoid hardening). The NaCl crystal should be white
and loose. After cooling, weigh it and calculate the yield.
2. Product inspection
Dissolve 1.0 g of crude table salt and purified salt (refined salt) in 5 mL distilled
water respectively, and then fill into three test tubes separately. Inspect their purity
by the following method.
(1) Inspection of SO42-: Add two drops of 1 mol/L of BaCl2 solution and two
drops of 2 mol/L of HCl solution to the NaCl solution before and after purification
respectively and observe the phenomena.
(2) Inspection of Ca2+: Add a few drops of 0.5 mol/L of (NH4)2C2O4
(ammonium oxalate) solution to the other two test tubes respectively. Observe the
phenomena and draw the conclusions.
(3) Inspection of Mg2+: Add a few drops of magnesium reagent to the remaining
two test tubes, and add 2 mol/L of NaOH solution if necessary.
According to the above experimental phenomena, compare the purity of NaCl
before and after purification.
[Questions]
1. What is the basis of the dissolution of 8.0g of salt by adding 30 mL of distilled
water? What are the effects of too much or too little water?
2. Why do we use BaCl2 to remove SO42- instead of CaCl2? Why do we use
NaOH and Na2CO3 to remove Mg2+ and Ca2+ instead of KOH and K2CO3? Why do
we use hydrochloric acid to remove the remaining OH - and CO32- instead of other
acid?
3. Why should we adjust the pH value to about 4 when using hydrochloric acid
to adjust the acidity of the twice filtrate?
4. Why should we not evaporate to dryness when purifying and concentrating
the purified salt solution?
[Expanding the Experimental Knowledge]

1. Magnesium reagent is an organic dye (p-nitrophenylazo resorcinol). It is
yellow in acidic solution and red-purple in alkaline solution, but it is sky-blue after
being adsorbed by newly formed Mg(OH)2 precipitation. Therefore, it can be used
to inspect the presence of Mg2+.
2. Solubility of NaCl and KCl
Table: Solubility of NaCl and KCl at different temperature
Temperature/℃ 0 20 40 60 80 100
NaCl/ (g/100g
35.7 36.0 36.6 37.3 38.4 39.8.
of water)
KCl/ (g/100g
27.6 34.0 40.0 45.5 51.5 56.7
of water)
3. Simple identification of table salt and industrial salt

Table salt whose main ingredient is NaCl is similar to industrial salt whose
main ingredient is NaNO2 in appearance and density. NaNO2 is a white or light
yellow crystal or powder with salty taste, much like table salt. Sodium nitrite is toxic
and a strong carcinogen. If people ingested 0.3-0.5g of sodium nitrite, they would
be poisoned and appear obvious poisoning status in 10 minutes after eating.
Moreover, it is seriously life-threatening.
The reaction of using NaNO2 to oxidize KI to produce elemental iodine under
acidic conditions:
2NaNO2+2KI+2H2SO4==2NO+I2+Na2SO4+2H2O
We can distinguish the sodium nitrite from the table salt because the elemental
iodine turns blue in the presence of starch.
4. Evaporation and concentration
We should carry out the operation of evaporation, concentration, and
crystallization when a substance precipitates crystals from the dilute solution. Pour
the dilute solution into an evaporating dish and heat slowly and stir continuously. So
the water in the solution is evaporated continuously and the solution is concentrated.
The crystal is precipitated by cooling when evaporating sufficiently. The degree of
concentration of the solution is related to some factors such as the solubility of the
crystallized substance and the change in solubility with temperature. If the solubility
of the crystallized substance was small or varied much with temperature, it would
be evaporated sufficiently when the crystal film appears. If the solubility of the
crystallized substance varied little with temperature, it should be cooled when being
evaporated to the porridge state. If it was desired to obtain large particles of crystals,
it should not be evaporated too much.
In the laboratory, the evaporation and concentration process is carried out in an
evaporating dish. The amount of the solution contained in the evaporating dish
should not exceed 2/3 of its capacity. Generally, when the thermal stability of the
substance is good, evaporation can be performed on the asbestos net, otherwise it
needs to be evaporated by being heated indirectly by water bath.
5. Formation of precipitation
In the case of purifying the substance, it is necessary to add the precipitant to
form the precipitate with the soluble impurity, and to remove it by filtration. How to
precipitate? The following circumstances need to be considered:
(1) Which kind of precipitation should be generated? Such as removing SO42- ,
we should consider which kind of precipitation SO42- could generate, PbSO4、SrSO4、
BaSO4、CaSO4、Ag2SO4 and so on. Among them, BaSO4 has the smallest solubility,
and after adding Ba2+, it can be removed in the subsequent operation without
introducing new impurity ions during purification.
(2) Add the precipitant according to the rule of solubility product. When the ion
product is larger than the solubility product constant, the precipitation can be
precipitated. When the precipitant is added more, the residual concentration of the
impurity ions is smaller due to the same-ion effect. However, it is not the more
precipitant, the better. When the precipitant is too much, the solubility of the
precipitation increases because the same-ion effect is masked by the salt effect
(sometimes there will be other side reactions), which is against the purpose of
removing impurities. Generally, the amount of the precipitant added may be 20% to
25% more than the required amount.
(3) The order of removing impurity ions Since an excess of 20% to 25% of the
precipitant is often added when the impurity ions are removed by precipitation. It
means that the solution contains an excess amount of precipitant, and it is necessary
to introduce new impurity ions when removing impurities. This is also the basis of
choosing the precipitant and the order of removing impurities.
(4) Conditions of precipitating in order to facilitate filtration, we hope that the
precipitated particles are larger. How can we get the large precipitated particles?
Add precipitant under the condition of heating. Then boil the solution for several
minutes. After the precipitation is complete, leave the precipitation and the solution
for a while, and these measures are good for the growth of the precipitated particles.
The placement process is called aging of the precipitant.
(5) Inspection of “whether the precipitation has completed or not” Before
filtration, we should inspect whether the precipitation has been complete or not. The
test method is that take a small amount of solution into a centrifuge test tube and add
2~3 drops of precipitant slowly to the supernatant solution after centrifugation.
Observe whether the precipitant is precipitated in the supernatant solution. If
precipitation occurred, the precipitation is incomplete, and the precipitant should be
added continuously. If precipitation didn't occur, the precipitation would be
complete and the following operations could be continued. Check whether the
precipitation is complete, which can also be carried out directly in the beaker. If the
precipitation in the beaker has settled at the bottom and the beaker wall is clear, the
precipitant can be dripped 2 to 3 drops along the wall of the beaker. Observe whether
the new precipitation is precipitated to determine whether the precipitation is
complete.

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Experiment 2: Purification of Sodium Chloride

[Apparatus, Medicine and Other Materials]

[Expanding the Experimental Knowledge]

3. Simple identification of table salt and industrial salt

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