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HCT 202:INORGANIC CHEMISTRY PART 11PRACTICALS

Compiled by Mambanda Isaac (Chief Technician) & Gonzo Muriel (Snr Lab Technician)

DEPARTMENT OF CHEMICAL TECHNOLOGY

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COURSE OUTLINE

The course is mainly designed to illustrate and reinforce the lectures on coordinating chemistry. It is mainly concerned with the d-block elements but some s and p-block chemistry is also involved.

During the course you will be introduced to the following instrumental techniques: Infra-red spectroscopy, visible/ultraviolet spectroscopy and magnetic susceptibility measurement, under no circumstances can you use the instruments involved without first having shown how to do so by the demonstrator.

Practical Write-up

You should ensure that the practical(s) started in any given week are completed, by the end of the second practical session. It is not necessary to copy out the methods already given for a preparation. On the reactions of an elect or compound should be recorded thus:

Test Observation Inference

All students must carry out the “reaction test” section of experiments 1-11 even though they may not be assigned certain with a reaction equation. All preparations should be described with a reaction equation. Also the yield of the experiments and the % yield should be given in the “Results” section. Dry samples should be handed in labeled tubes with your name, date, name of compound and yield written on the label. A discussion section should answer any questions specificically asked and include any conclusions you might reach. All write-ups must be in hard covered note books with your name clearly printed on the outside.

Each practical will be marked out of 50 taking into account, write-up, yields, discussions and conclusions. Do not copy sections out of text books but explain things clearly in your own words.


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EXPERIMENT 1:

(d-block elements – Titanium)

Reactions of titanium ( IV) and (III) compounds

Record all observations and interpret them as far as possible.

A. Titanium (IV) ( Using 15% titanium (IV) chloride in hydrochloric acid)

1. What are the species present in the solution?

2. Add about 5cm3 of the 4M NaOH solution to about 2cm 3 of the test solution. What is the product of the reaction?

3. Repeat 2 but using concentrated NaOH and warm gently.

4. Repeat 3 but using 1:1 ammonia solution.

5. Pass SO2 gas through 2cm3 of solution.

6. Add a little zinc dust to about 2cm3 of solution. Compare with reaction 4.

7. Add a few of test solution to about 2cm3 of water then add a drop of 6% hydrogen

peroxide. Now add a little solid sodium fluoride and shake. What are the products of the reaction.

B. Titanium (III) ( Using dilute titanium ( III) (chloride in hydrochloric acid)

1. Repeat tests 2 and 3 from A.

2. Add dilute potassium permanganate solution dropwise.

3. Prepare a concentrated solution of sodium perchlorate. Warm and add a few drops of the of solution.

4. Add a few drops (of test solution to ammonia ferric sulphate solution.

5. Record the visible/ ultra-violet spectrum of dilute aqueous titanium (III) chloride Solution using a 1 cm cell.

Determine the position of maximum absorption and hence calculate the crystal field splitting energy for Ti3+ in an octahedral environment of water ligands in the mol-1.


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EXPERIMENT 2 ( d-block elements – Vanadium)

(A) Reactions of Vanadium

Suspend about 0.5g ammonium metavanadate NH4VO3 IN 5cm3 of water and 5cm3 dilute sodium hydroxide. Dilute to 25cm3

and use this for tests. Record all observations and interpret them as far as possible.

1. Slowly add 2M HC1 to 1cm3 for the solution until it is in a large excess. Explain the observed color changes in terms of the species present in solution.

2. Acidify the solution with dilute H2SO4 and pass hydrogen sulphide gas.

3. Pass sulphur dioxide gas through the solution

4. Acidify with dilute HCI and add a piece of granulated zinc. Observe the changes which take place over 30 minutes.

5. Acidify the solution (2cm3) with 2cm3 4H H2SO4, then add a few drops of 20 vol hydrogen peroxide. Observe any reaction that has occurred and then add an excess of solid sodium fluoride (1g). Explain your observations.

6. The following tests are carried out using solid NH4VO3

(i) Add a little of the solid (0.2g) to a concentrated HCI (2cm3).(ii) Strongly heat the solid (2g) in a nickel crucible. What is the product?

Attempt to dissolve it in concentrated HCI and explain any reaction observed.

(B)Preparation of a vanadium (IV) complex with acetyl acetone (2.4- pentanedione

Cautiously add concentrated H2SO4 (10cm3) to an equal volume of water. Then add ethanol (25cm3) and vanadium pentoxide (5g). Reflux for 1-2 hours until the solution changes from green to blue. Filter off the solid using a Buchner funnel and add 13cm3 acetyl acetone to filtrate. Neutralize the solution by adding 20g anhydrous sodium carbonate in 125cm3 water. Filter the product and dry in air. Recrystallize from chloroform.

(i) The formula of the product is VO ( acac)2. Name and draw the structure of the complex.

(ii) Record the yield and calculate the percentage yield of the reaction.


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(iii) How would you expect the compound to react with pyridine? Give the structure

of the expected product.

C. Preparation of titanium (IV) complex with acetyl acetone (2.4 pentanedione)

To 10cm3 glacial acetic acid add 1cm3 acetic anhydride and 3.2cm titanium (IV) chloride. Cool in ice and add 6cm3 actylacetone. Boil (bin a fume cupboard using a hot plate naked flame) carefully and not cooling, a red-yellow crystalline precipitate forms. Filter off the crystals using a Buchner funnel and wash with Petroleum ether (B.P. 60-800C).Recrystallise from boiling acetic anhydride mixture (12:1)

i. Record the yield. Name the compound.ii. Calculate the percentage yield obtained.

iii. The formula of the product is Ti (acac)2 Cl2

Could it exist in more than isomeric form? If so, also show the different isomeric forms.

D. Devise and then carry out a volumetric method of determining the molarity of Ti3+

in the titanium (III) chloride solution provided.


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EXPERIMENT 3

(d-block elements- chromium )

A. Reaction of chromium

Record and interpret all observations

Using an (approx) 5% aqueous solution of chrome alum K[Cr(H2O)5][SO4]2.6H2O for tests.

1. Slowly add 4M NaOH to the test solution (2cm3) until no further reaction takes place. Explain the observed reactions.

2. Repeat 1, using 4M aqueous ammonia. Compare the results with those obtained in 1.

3. Mix the test solution (2cm3) with an equal volume of 4M HC1 and add a little zinc dust. Heat the solution until hydrogen is freely evolved. Note any colour changes. Decant the supernatant liquid into a stirred concentrated solution of sodium acetate. Explain the reactions involved.

4. To the test solution (2cm3) add a little solid ammonia peroxodisulphates and boil. Explain the observed changes.

5. Using (approx) 5% aqueous chromium (III) chloride as the test solution. Mix the test solution (2cm3) and add a little zinc dust. Heat the solution until hydrogen is freely evolved. Cool and rotate the tube to spread the solution in a layer over the wall. Note and explain the colour changes.Using (approx) 5% potassium dichromate as the test solution.

6. Add a few drops of sodium hydroxide solution to the test solution.

7. Add hydrogen peroxide solution dropwise to the test solution.

8. Repeat 7 using an alkaline test solution.

B. Preparation of compounds of chromium (III)

(i) Potassium trioxalatochromate (III0 trihydrate


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Add 9g of Oxalic acid crystals, H2C2O4, 2H2O, to 20ml of water at about 700C. Stir well and add small quantities of powdered potassium dichromate using a total of 3g of this reagent. When the reaction has subsided, boil the resulting solution and add 3,5g of potassium oxalate monohydrate. K2C2O4, H2O. Allow this to dissolve before cooling the mixture to room temperature. Add some 3-4ml ethyl alcohol and continue cooling the mixture in an ice bath. Blue-green crystals of the salt separate from a dark solution. An additional small volume of alcohol may be added to the solution if difficulty is experienced in initiating crystallization. Filter off the crystals using either a small Bunchner or Hirsch funnel or a small Buchner flask. Wash the product with a small volume of hot pure ethyl alcohol. Drain and dry the crystals in the usual manner using the filtration apparatus. Record your yield.

(ii) Potassium cis-dioxalatodiaquachromate (III) diyhdrate

Carefully reduce to fine powders in a dry mortar 12g of oxalic acid crystals, H2C2O42H2O. Then add 4g potassium dichromate. Mix the powders carefully in the mortar before transferring to an evaporating dish that has been previously moistened. It will be found advisable to form a compact heap of the powder in the center of the dish. Cover the dish with a large watch-glass and warm the dish on a low-temperature hot-plate. A vigorous reaction occurs and spread throughout the mixture. This results in the formation of syrup. Continue to warm the dish and add 20ml ethyl alcohol. Triturate the product of the reaction until it solidifies. Sometimes, it is helpful to decant the liquid and replace it with fresh alcohol (20ml) if solidification does not occur easily. The alcohol must be warm and the product titrated with a normal size spatula to obtain a granular crystalline product. Filter and dry the product. Record your yield. Note the cis-form of this complex oxalate appears almost black in diffuse daylight or deep purple in artificial light. Its solution is a red-purple colour in transmitted light.

(iii) Potassium trans-dioxalatodiaquachromiate (III) trihydrate

Dissolve 12g oxalic acid crystals in the minimum volume of boiling water in a 400ml beaker. Add a solution dichromate in the minimum volume of hot water. This addition must be carried out using small portions of hot dichromate solution. The beaker should be covered with a watch-glass during the violet reaction that follows each addition. Cool the beaker and its contents and transfer the solution to a large crystallizing dish (10cm diameter). Cover the dish and set on one side for 46 hours. During this period the solution should be able to evaporate to about one-third of its original bulk, and deposit crystals. Collect the crystals on a small Buchner or Hirsch funnel in the usual way. Wash them several times with small volumes of cold water and finally with alcohol. Drain and dry the crystals in the usual manner. Record your yield. Note the trans-form of this complex oxalate is rose-coloured.


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EXPERIMENT 4

(d-block elements- Manganese)

Reactions of Manganese

Use a 5% solution of Manganese (II) sulphate for the following test 1 and 2.

1. Add 4M NaOH solution (2cm3) to the solution and allow to stand for ten minutes. Explain the reactions.

2. Repeat test 1. Then add a (2cm3) of 20 vol hydrogen peroxide Filter, wash the precipitate then heat with dilute HCl. Test for chloride evolution.

3. Dissolve KOH (1g) in water (3cm3). Add manganese (IV) oxide 0.1g and heat the suspension. Explain the reaction.

4. Repeat test 3.Using potassium permanganate.

5. Add freshly prepared iron (II) sulphate solution (or F.A.S) in excess to (approx) 1cm3 of dilute potassium permanganate solution acidified with 2M H2SO4Compare his reaction with the reaction which occurs when excess iron (II) sulphate or (F.A.S) is added to approximately 1 cm3 of potassium permanganate to which one drop of 2M NaOH has been added.

C. Preparation of Manganese (III) compound

Dissolve manganese (II) chloride tetrahydrate (2.5g) and sodium acetate trihydrate (7.5g) in water (100cm3), and to the stirred solution add slowly acetylacetone(10.5cm3). Treat the resultant two phase system with potassium permanganate solution (0.5g in 25cm3of water); after a few minutes add in small amounts with stirring, sodium acetate solution (7.5g in 25cm3 of water). Heat the solution to about 600C for 10minutes, cool in ice cold water and filter at the pump. Wash with ice cold water and small quantities of acetone to facilitate drying. Dry at the pump.

1. Record the yield2. Calculate the percentage yield based on the manganese (II) chloride tetra

hydrate.3. What is the role of KMnO4 in the reaction?4. Why is it necessary to add sodium acetate?5. The formula of the complex is Mn (ac.ac)3. What is its structure and does

the structure have any isomeric forms, if so, what are they?


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D. Complementary work

1. Dissolve a small amount of the complex in water and allow to stand for a few minutes.Note what happens and explain the reactions.(a) Analyse the compound for manganese by reducing the cation to manganese

(II) with iodide. Weigh accurately a sample of the compound (0.4g) and add 2M NaOH (25cm3).Heat the mixture on steam bath the suspended solid.


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EXPERIMENT 5

(d- block elements- cobalt)

1) Reactions of cobaltUse an = 1M solution of cobalt (II) chloride or nitrate

a) Add concentrated sodium hydroxide. Does the precipitate dissolve in excess? Add hydrogen peroxide.

b) Repeat test (a) using ammonia hydroxide

c) Add excess concentrated solution followed by a little acetone divided into four parts.

d) Add ammonium thiocyanate solution followed by a little acetone. Divide into four parts:1. Shake part with a little ether

2. To part add a little mercuric chloride solution and boil

3. To part add a small amount of solid ammonium fluoride.

4. Record the visible spectrum of part of the solution and compare it with that of cobalt (II) chloride solution.

e) Add potassium nitrite solution and acidify with dilute acetic acid.

f) Add a little solid potassium nitrite and bubble air through the mixture.


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Preparation and Properties of (-)-[Co (en)l3 l3.H2O

IntroductionCertain classes of coordination compounds can exist in a number of isomeric forms. This assignment deals with the optical isomers and an octahedral complex in which three identical chelate ligands occupy the six coordination sites around the central metal stom.

Aim1. To study the preparation of the dextro- isomer of an octahedral chelate

complex and measure its optical activity. 2. To become aware of the properties which enable a resolution of isomers to be

made3. To scale down a published experiment method

Experimental

1. Prepare 2g of dextro-tris (ethylenediamine) cobalt (III) iodine monohydrate.2. Measure the specific rotation of both the diateroisomer and the resolved (+)-

isomer using a POLARIMETERNote: - Ethylenediamine (en) is also known as 1,2 diaminoethane.

B PREPARATION OF IRON (II) OXALATE AND POTASSIUM TRIOXALATO FERRATE (II) TRIHYDRATE

Method

A Iron (II) oxalate

Dissolve ferrous ammonia sulphate (15g) in warm water (50cm3) which has been acidified with 2M sulphuric acid (1cm3). Add a solution of 10% Oxalic acid (75cm3) with rapid stirring. Gently heat the mixture to the boiling point and then allow the yellow precipitate of iron (II) oxalate to settle. Remove the precipitated by filtration on a Buchner funnel. Wash it thoroughly with hot water and then with acetone. Allow the product to dry on the Buchner funnel. Weigh it on a rough balance and then divide into two equal portions.

B Potassium Trioxalatoferrate (III) Trihydrate

Suspend one portion of the iron (II) oxalate in a warm solution of potassium oxalate (5g in 15cm3 of water) Add 20 vol hydrogen peroxide (12.5cm3 from burette whilst the solution is stirred continuously and maintained at 40oC. The solution now contains a precipitate of ferric hydroxide. Remove this by heating


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the solution to boiling; add 10% oxalic acid (about 3cm3) dropwise from a burette until the precipitate just dissolves. During the addition of oxalic acid the solution should be maintained near the boiling point. Filter the hot solution. Add ethanol (15cm3) to the filtrate, redissolve any crystals formed by gentle heating and put the solution in a dark cupboard to crystallize. Remove the crystals by filtration on a Buchner funnel. Wash them with an equivolume mixture of ethanol and water and finally with acetone. Weigh the product on a rough balance. The complex is photo- sensitive, but it is quite stable if it is stored in the dark.

Analysis of Iron (II) Oxalate for Iron and Oxalate

Dissolve the oxalate 0.3g. (Accurately weighed) in 2M sulphuric acid (25cm3). Heat the solution to 60oC and titrate with the standard (0.02M) potassium permanganate solution until the first permanent pink colour. Add zinc dust (2.0g) to the solution and boil it for 25minutes. Filter through glass wool and wash the residual zinc with 2M sulphuric acid. Add the washings to the filtrate and titrate this solution with standard potassium permanganate as described above. Repeat the analysis.

EXERCISE

1) Determine the percentage of iron, oxalate and water in the iron (II) oxalate and derive its empirical formula.2) Write balanced reaction equations for both preparations and calculate the percentage yields of both products.3) Suggest a possible structural formula for iron (II) oxalate4) Draw the possible isomers of potassium trioxalatoferre (III). Hand in labeled samples of both products with your written work.

Reference

Inorg. Synth. 1960., 6 186

Notes

1.Dont forget to show reaction schemes, yields theoretical values, molecular weighs etc.

2.Some aspects of symmetry should be mentioned in your discussion.

3.Water of crystallization cannot be ignored. (Adams and Raynor, p163)

4.The discussion of your results should include brief details of the reaction scheme and mechanism which may require the use of additional references such as Cotton & Wilkinson and Mackay and Mackay. These should be included in the


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text as appropriate and where possible the original papers should be consulted. (Note, optical isomerism is often discussed in organic text books.)

Preparation and Resolution of the Tris (ethyleneodiamine) cobalt (III) Iron

Preparation and resolution of the Tris (ethyleneodiamine) cobalt (iii) IronThe tris (ethylencoiamine) cobalt iron is an example of a complex cation that exhibits optical isomerism, and when it is prepared a racemic mixture of d and 1 forms obtained. In this experiment these two antipodes are separated by fractional crystalisation of their tartrates.

Materials required:

Cobalt (ll) sulphateConcentrated hydrochloric acid2mol /dm3 hydrochloric acidBarium hydroxided-Tartaric acidActivated charcoalConcentrated aqueous ammonia

Mix ethylenediamic (13.2cm3)and water (30cm3) in a Buncher flask and cool this solution in an ice bath. Add to the solution concentrated hydrochloric acid (11cm3), cobalt sulphate (916.8g) dissolved in cold water (30cm3) and activated charcoal (2.5g). Draw a rapid stream of air through the solution (Fig 11) for 4hrs and then adjust the pH to 7-7.5 (using wide-range indicator paper) by the addition of 2mol hydrochloric acid or ethylene diamine as required heat the solution on a stem both for 20min, cool and remove the charcoal by filtration. Wash the charcoal with hot water (15cm3) and add the washes to the filtrate which is a solution of tris (ethylene diamine) cobalt chloride sulphate. Prepare a solution of Barium tartrate by mixing solutions, Barium hydroxide (18.8g) and d-tartaric acid (9.0g) (both dissolve in the minimum quantity of water) at 90oC. Cool the solution. Collect the product by filtration and wash it on the filter with warm water. Add the solid barium d-tartrate to the tris (ethylene diamine) Cobalt (lll) chloride sulphate solution and heat the mixture on a boiling water bath with constant stirring for 30minutes. Remove the precipitated barium sulphate filtration and wash it with hot water (10cm3). Add the washing to the filtrate and evaporate this solution to 35cm3. Allow the solution to stand at room temperature for approximately 15h during which time red crystals of (+) tris (ethylene diamine) cobalt (lll) chloride d-tertrate pentahydrate are formed. Collect these crystals by filtration and keep the filtrate A which contains the (-) isomer. Wash the crystals with an equivolume mixture of ethanol and water (15cm3), then absolute ethanol (10cm3) and dry in a vacuum.

Preparation of (+)Tris (ethylene diamine) cobalt (III) iodine hydrate dissolve the (+) tris (ethylene diamine) cobalt (III) chloride d-tartrate in hot water (12cm3) and to the stirred


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solution and concentrated aqueous ammonia (0.3cm3) followed by a solution of sodium iodide(20.4g) dissolved in hot water (8.5cm3). Cool the solution in an ice bath, collect the product by filtration on a Buchner funnel and wash it on the filter with an ice cold solution iodide (3.5g) in water (12cm3) and then acetone. Dry the product on the filter by maintaining the vacuum, and record the yield.

Exercises

1) Measure the optical rotations of the three resolved complexes in the following manner, using a polarimeter. It is assumed in this discussion that the polarimeter with a sodium lamp (sodium-d line 589.3nm) according to the instructions of the instrument. Place an empty tube in the polarimeter and determine the null point; that is, when the two halves of the field of view are of equal intensity. Prepare accurately a 2-3% solution of each isomer under investigation and place it i the sample tube in the polarimeter. (A solution of this concentration should give a polarimeter reading of several degrees). Then adjust the analyzer so that the two halves of the field of view are of equal intensity. The difference between this reading and that obtained at the null point is the angle of rotation for the solution. Repeat this determination until consistent results are obtained. Measure the temperature of the solution at which the measurements were made and calculate the specific rotation.

The concentration of the optical isomer in g/100cm3 of solutionThe length of the column solution in decimetersThe frequency if the light used for the measurementThe temperature in OC of the sample on which the measurement was made.

Discussion

1. Illustrate how this complex can exist as optical isomers

2. Which chemical factors enable two such structurally similar compounds to be isolated?

3. Complex formation can bring about the stabilization of valency states transition metals other than those commonly found? Comment on this statement with reference to this experiment.


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EXPERIMENT 6:

(d-block elements-iron)

Reactions of iron (II) and (III) compounds

Use ammonium iron (II) sulphate for reactions of iron (II). Use iron (III) nitrate solution for reactions of iron (III)

1. Add excess 4M NaoH solution to approximately 2cm3 iron (II) solution.

2. Repeat 1 but use ammonia solution instead. Compare the two results.

3. Repeat 1 but use sodium carbonate solution. Compare with reaction in 1.

4. Repeat 1, 2 and 3, but using iron (III) solution.

5. Add excess ammonia thiocyanate solution to iron (II) and iron (III) solutions.

6. Divide the iron (III) solution from 5 into two portions then add:-

(x) A little ammonia fluoride.

(y) Tin (II) chloride solution.

7. Add excess potassium iodide solution to approximately 1cm3 of iron(III) solution, followed by sodium thiosulphate solution until the mixture is colourless. Now add a drop of ammonia thiocyanate solution. Comment on the reactions occurring.

8. Add a drop of bromine water to approximately 1cm3 of a iron (II) solutions. Then a drop of ammonia thiocyanate solution. From reactions in 7 and 8 estimate the range within which the oxidation potential for Fe2+, Fe3+ must lie.

9. To FeCl3 . 6H2O (2.7g) in water is added acetylacetone (3g) followed by sodium acetate hydrate (4g) dissolved in 20cm3 water. After warming for a few minutes the precipitate is filtered off and recrystallised from absolute ethanol.

i. Test and explain the solution of the compound in water and diethyl ether.

ii. What is the role of sodium acetate I the reaction?

iii. Draw the structure of the compound


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EXPERIMENT 7:

(p-block elements, Group IV)

For the following tests, use solutions of sodium silicate, stannous chloride, stannic chloride, lead acetate with red lead (dissolved in boiling dilute nitric and filtered- Pb(IV).Explain all observations.

(1) Pass hydrogen sulphide into solution of :-

(a) Sodium silicate(b) Acidified stannic chloride(c) Acidified stannous chloride(d) Pb (IV) solution(e) Acidified led acetate

(2) Add 1cm3 ferric chloride solution to a solution of:-

(a) Stannous chloride

(b) Lead (II) acetate. Add to the resulting solutions one drop of potassium hexacyanoferrate (III) solution.

What conclusions can you draw from (1) and (2) concerning the relatives stabilities of various oxidation states?

(3) Place about 10cm3 of anhydrous tin (IV) chloride in a test tube and carefully add 2M sodium hydroxide. Repeat the procedure with 4M HCl.

(4) Place about 2cm3 of water in a test tube and carefully add 1cm3 of tin 9IV) chloride: Cool to 00C

How do reactions (3) and (4) compare with the corresponding reactions of carbon tetrachloride?

Preparation and analysis of Tin (IV) iodide

Mix 3g of stannous chloride crystals (SnCl2.2H2O) with 25cm3 of equivolume mixture of glacial acetic acid and acetic anhydride in 100cm3 ‘Quickfit’ flask. Boil the mixture under reflux for 15 minutes. To dehydrate the stannous chloride. Allow the solution and precipitated anhydrous stannous chloride to cool a little and while shaking the flask add 3.3g of iodine down the condenser in portions. The cream coloured precipitate formed


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first is dichlorodi-iodotin (SnCl2I2).This redissolves as the last portion of iodine are added.

When the iodine has been added, reflux the solution for a few minutes to the reaction and allow it to cool. Stannic iodide will come down as small orange crystals, while the chloride remains in solution. Filter off the solid RAPIDLY by suction (stannic iodide is hydrated by the moisture in the air) and recrystallise it immediately from a small quantity of chloroform. Weigh.

Percentage of Iodine in Stannic Iodine

Weigh a sample (about 0.25g ) into a glass stoppered flask: add 30cm3 of concentrated hydrochloric acid and a few cm3 of chloroform of carbon tetrachloride. Titrate with a standard solution of potassium iodate (containing about 1.25gin 250cm3) until on vigorously shaking the flask, the violet coloration in the organic layer just disappears (the aqueous part will be pale yellow).the first action of the iodate is to oxidize the iodide. This is then oxidized further to iodine monochloride (ICI) which, as the anion ICI2,gives the final aqueous layer its yellow colour. Write down the equation for the two oxidation steps, and hence deduce that KIO3 is equivalent to 2I. Compare the percentage iodine you obtain with that required for formula SnI4 981.05%). What are the products when SnI4 and with 1.1 and 1.2 proportions of pyridine.

Complementary work (Comment on all observations)

1. Prepare a solution of tin(IV) iodine in acetone (5cm3) and divide it into two portions and B. To A add a few drops of water. To B add similar quantity of saturated potassium iodine solution.

2. Comment on the colour difference of tin (IV) chloride and tin (IV) iodine.


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