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Hands-on Chemistry

 Michon
 
 

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 International Year  of Chemistry - 2011

Hands-on Chemistry
 Beaker  Beaker


(2011-07-31)  
The contents of the chemistry set I had as a child  (if memory serves).

A chemistry set should be fun but it should also serve asan initiation to safety procedures. Here is the list of the basic equipment in the chemistry set whichI learned to use safely as a child.

  • Glass stirring rod.
  • Round-bottom and flat-bottom boiling flasks.
  • Verres à pied  (no beakers).
  • One-hole and two-hole stoppers.
  • Thistle funnels and glass tubes.
  • Retort
  • Mortar and pestle.
  • Evaporating dishes.
  • Crucible.
  • Tripod and wire gauze  (with asbestos center).
  • Alcohol burner with wick.
  • Test tubes and wooden rack.
  • Wooden test-tube clamp.
  • Test-tube cleaning brush.
  • Plastic crystallizers  (one with built-in electrodes).
  • Earthenware gizmo  (pierced bowl with sideways indentation).
  • Litmus paper  (French: papier de tournesol ).

Two wooden racks were provided with small quantities of inorganic andorganic chemicals in labeled glass tubes with plastic stoppers. Some of those tubes were empty, probably because their intended content was deemedtoo dangerous  (lye)  or too expansive  (silver nitrate). The silver nitrate container was darkened.

  • Iron filings.   Fe   55.845 g/mol.
  • Sulfur.   S   32.065 g/mol.
  • Zinc dust.   Zn   65.379 g/mol.
  • Pyrolusite = Manganese dioxide.   MnO2   86.937 g/mol.
  • Condy's crystals = Potassium permanganate.  KMnO4
  • Sodium bisulfite.   NaHSO3
  • Copper sulfate.   { CuSO4, 5H2O }   249.685 g/mol.
  • Lunar caustic =Silver nitrate  { AgNO }   169.873 g/mol.
  • Baking soda =Sodium bicarbonate.   NaHCO3
  • Washing soda =Sodium carbonate.   Na2CO3
  • Caustic potash.   KOH   56.106 g/mol.
  • Lye = caustic soda = sodium hydroxide.   NaOH   39.997 g/mol.
     
  • Glucose.  H(CHOH)5HCO   180.156 g/mol.
  • Oxalic acid.  { (COOH)2, 2HO }   126.066 g/mol.
  • Citric acid.  { (CHCOOH)COH COOH , HO }   210.139 g/mol.
  • Tartaric acid.  { (CHOH COOH)2 }   150.087 g/mol.
  • Malic acid.  { COOH CH2 CHOH COOH }   134.087 g/mol.

A few other common compounds may provide a slightly richer playfield:

  • Table salt =sodium chloride.   NaCl   58.442 g/mol.
  • Epsom salt =magnesiumsulfate.  { MgSO4, 7H2O }  246.475 g/mol.
     
  • Table sugar = sucrose =saccharose.   C12H22O11   342.297 g/mol.
  • Fruit sugar =fructose.   C6H12O6   180.156 g/mol.
  • Galactose.   C6H12O6   180.156 g/mol (vs. glucose & fructose).


 Aspirator bottle (2011-07-10)  
Handling liquids  (and gases).

  • Test tube.  Boiling tube  [ tube à essai ].
  • Stirring rod  [ agitateur ].
  • Crystallizer, crystallizing dish  [ cristallisoir ].
  • Petri dish  [ Boîte de Petri ].
  • Watch glass  [ Verre de montre ].
  • Measuring cylinder  [ éprouvette graduée ].
  • Volumetric flask  [ fiole jaugée ].
  • Buret  [ burette ].
  • Pipet  [ pipette ].
  • Thistle funnel, thistle tube.
  • Separatory funnel  [ ampoule à décanter ].
  • Dropping funnel  [ ampoule de coulée ].
  • Pressure-equalizing dropping funnel  [ ampoule à brome ].
  • Eudiometer  (Landriani, 1775).
  • Aspirator bottle  (bottom side-arm).
  • Bottle  [ flacon ].
  • Squeeze bottle  [ pissette ].
  • Round-bottom flask, Boiling flask, Florence flask  [ ballon ].
  • Flat-bottom flask.
  • Beaker  [ bécher ].
  • Conical flask (Emil Erlenmeyer, 1861).
  • Filter flask, side-arm vacuum flask, Büchner flask, Kitasato flask.
  • Büchner funnel  (with either filter paper or sintered/fritted glass).
  • Büchner ring.
  • Desiccator jar.
  • Water aspirator  [ trompe à eau ].
  • Retort[Cornue ]  (Geber, c. AD 750).
  • Alembic, still [ alambique ].
  • Liebig (straight) and Graham (coiled) condensers  [ réfrigérants ].
  • Kjeldahl bulb  (or "ball").
  • Bump trap  (reflux trap).
  • Rotary evaporator  (or "rotovap").  [video |MIT|use ]


(2011-07-12)   (Teflon®)
(CF2)n  was discovered accidentally by Roy J. Plunkett  in 1938.

On April 6, 1938, Plunkett and his assistant, Jack Rebok, found that asteel cylinder in which they had storedtetrafluoroethylene  (TFE) contained a waxy powder instead  (they had to cut the cylinder open). The compressed gas had spontaneously polymerized into PTFE.

PTFE  has a very low friction coefficient  and is virtually inert chemically.

 Come back later, we're still working on this one...


(2011-07-12)  
Ground-glass joints, hose connections, etc.

Ground-glass conical joints

In the trade, the inner contact surface is known as the grind.

All standard joints have a precise 1:10 taper.  Their sizes are specified bytwo numbers; the largest diameter of the grind  (in mm) and the length of the grind  (in mm). A mismatch in length is usually inconsequential. A  slight  diameter discrepancy can also be tolerated. The 10/30 long joint seems to be for thermometers only...

Sizes (diameter/length in mm) of Ground-Glass Conical Joints
Keck
Clip
 Size Wall
Thickness
US
  (long)  
DIN
  12249  
Other
  (short)  
  3.5-5.0 mm  100/60
  3.5 mm  85/55
  3.2 mm  71/51
  2.5-3.2 mm  60/46
  2.5-3.2 mm55/50 55/44
  2.3-2.5 mm50/50 50/42
brown 2.3-2.5 mm45/5045/40 
gold62.0-2.3 mm  40/38
orange52.0-2.3 mm34/4534/3534/28
red42.0 mm29/4229/3229/26
green31.8-2.0 mm24/4024/2924/25
blue21.8 mm19/3819/2619/22
yellow11.5-1.8 mm14/35,14/2014/2314/19
violet 1.5-1.8 mm12/3212/21 
  turquoise  0  thermometer  10/30  
1.5 mm10/3010/19 
  1.5 mm7/257/16 
  0.8 mm5/205/13 

Keck clips  were patented in 1984 (US patent4,442,572) by Hermann Keck. They are available mostly for medium-sized glassware joints  (10 mm to 45 mmin diameter)  in the above Delrin® color coding.

 Come back later, we're still working on this one...

 Bottom of the meniscus in a buret
(2011-07-11)  
Measuring volumes and concentrations.

Titration  is an elementary method of analytical chemistrywhich consist in measuring what volume a known titrant (or titrator)  solution should be added to an unknown solutionfor an observable reaction to occur. Often, what makes the reaction observable is the addition to the unknown solutionof a minute quantity of a color indicator  which changescolor under precise conditions.

Three type of titrations are based on color changes brought about, respectively,by a change in acidity, oxydizing potential or the concentration ofcomplexified metal cations. A related fourth type of titration is based on the observation of the precipitationof a sparingly soluble  specific solute.

1.   Acid-base titration :

This is the most common form of titration;it serves as an introduction to the subject at the high-school level. Student are introduced topH indicatorsand trained in the basic titration techniques, using aburette.

2.   Redox titration :

A spectacular introduction is the blue bottle demonstration.

3.   Complexometric titration :

complexometricindicator  (also known as a "pM indicator", where "M" stands for "metal") changes color as it forms a weak complex with a specific metallic cation.

4.   Precipitation titration :

 Come back later, we're still working on this one...


(2015-07-18)  
Solutes whose colors depend on the acidity of the solution.

An acid-base color indicator is a substance which undergoes a reversible color change with varying pH. Substances that undergo an irreversible  color-changing degradationabove or below a certain pH can be used to spot-check an existingacidity level, but they are not  proper indicators.

Most commonly, a pH  color indicator is a weak acid  HA  (of dissociation constant Ka ) which differs in color from its conjugate base A 

[ H+]  [ A/  [ HA ]   =   Ka

Somewhere in the color transition range  (exactly where depends onthe optical characteristics of the two colored species) there's a point where the two conjugate concentrations are equal. At that point, we have:

pH   =   pKa

Some weak acids undergo multiple color changes at different pKa  values.

Color transitions of some  pH indicatorsRoman numerals indicate multiplicity.
NameFormulaAcidicLowpKaHighBasic
Thymolphthalein (I)Red0.0Colorless
Phenolphthalein (I)Orange0.0Colorless
Picric acid (TNP)Colorless0.20.381.0Yellow
Cresol red (I)Red0.21.01.8Yellow
Crystal violet 10BYellow-1.01.151.6Violet
Phenol red (I)Red1.2Yellow
Malachite green (I)Yellow0.21.301.8Green
Thymol blue (I)Red1.21.652.8Yellow
Methyl greenYellow2.03.0Blue
Quinaldine redColorless1.32.633.2Red
Methyl violet 2BYellow0.152.1?3.2Violet
Methyl yellowRed2.93.34.0Yellow
Methyl orangeRed3.13.464.4Yellow
Bromophenol blueYellow3.03.854.6
Congo redBlue3.04.15.2Red
Helianthine (??)Orange3.45.0Pink
Bromocresol greenYellow3.84.85.4Blue
ResazurinOrange3.86.5Violet
Methyl redRed4.44.956.3Yellow
Propyl redRed4.85.486.6Yellow
Azolitmin (Litmus)Red4.58.3Blue
Chlorophenol redYellow5.06.256.7Red
Bromocresol purpleYellow5.26.356.8Purple
p-NitrophenolColorless5.47.157.6Yellow
Neutral redRed6.87.28.0Amber
Bromothymol blueYellow6.07.307.6
Phenol red (II)Yellow6.87.78.2Fuchsia
Curcumin (Turmeric)Yellow7.47.88.6Red
m-NitrophenolColorless6.88.288.6Yellow
Cresol red (II)Yellow7.18.468.8Purple
Thymol blue (II)Yellow8.09.209.6Blue
o-CresolphthaleinColorless8.29.619.8Violet
Phenolphthalein (II)Colorless8.39.710.0Fuchsia
Thymolphthalein (II)Colorless9.310.110.5Blue
Alizarin yellow RYellow10.111.012.0Red
Trinitrotoluene (TNT)Colorless11.213.0Orange
Indigo carmineBlue11.412.213.0Yellow
Phenolphthalein (III)Fuchsia12.013.0Colorless
Malachite green (II)Green11.613.2Colorless
Titan yellowYellow12.213.2Red
1,3,5-TrinitrobenzeneColorless12.014.0Orange

Before the invention of digital pH-meters, there were many more color indicators to choose from. Eastman-Kodak  alone was once offering up to  67  different indicators (Ellen McCrady,1995).

Litmus :

The oldest indicator of acidity still in use is Litmus, which was discovered around 1300 by the Catalan physician Arnau de Vilanova (c.1240-1311).

 Augustin Pyrame de Candolle (1778-1841) Traditional litmus  (CAS 1393-92-6) is a mixture of about a dozen substances extracted from Roccella tinctoria (Orchilla weed, described by Pyrame de Candolle  in 1805) or,  more recently, other lichens (which are also the source of Orcein). Such dyes have been known generically, sinceancient times,as lichen purple.

Litmus  was first analyzed in 1840 by the Irish chemist SirRobert Kane  (1809-1890). The main constituents of commercial litmus are:

Natural Indicators :

Besides litmus,  severalplant extractsare noteworthy for historical reasons:

Red-cabbage juice :  The active ingredients are anthocyanins which are the pigments that make red-cabbage purple, poppies red and cornflowers blue. Arguably, this is the most readily available pH indicator. Its multiple active components induce several color transitions.

Red-beet juice :  There are no anthocyanins in red beets. Thesingleactive dye is betanin  (E162, Beetroot red) at a concentration of about  500 mg/kg  (0.05%). It changes from red to yellow between pH 11 and pH 12.

Turmeric :  The active dye is curcumin (E100, Turmeric yellow)  which is also a redox indicator. It gives its yellow color tocurry  (curry contains turmeric). Curcumin is yellow below  pH 7.4  and red above  pH 8.6.

Red carmine :  Carminic acid () is the active constituent (12%) in cochineal  powder, obtained by grinding the bodies of dried female cochineal insects (Dactylopius coccus) mixed with aluminium or calcium salts. It takes about 70000 insects to obtain a pound of cochineal  powder, containing about 50 grams of carminic acid. This was a substantial trade in Mexico during Spanish colonial times. Renewed interest in natural dyes has made the product profitable againfor cosmetics  (Peru is now the leading exporter). Carminic acid  (CAS 1260-17-9)  has a pKa of  3.13 (2010). Yellow in acid, it has a deep violet color in an alkaline solution.

Universal Indicators :

Universal indicators  are just mixtures ofseveral simple indicators from the above list,carefully chosen to produce different colors in successive ranges covering a large part of the pH spectrum. The most popular universal indicators give the illusion of takingon a color varying continuously from red  (very acidic) to violet  (very alkaline)  like thecolors of the rainbow.

  • Yamada's Universal Indicator (1933).
  • Bogen's Universal Indicator.


(2015-08-13)  
The classic blue bottle  demonstration.

 Come back later, we're still working on this one...

More recently, another more colorful version of the same demonstration has becomepopular.  By using indigo carmine instead of methylene blue  the different stages areindicated by three different colors  (red, yellow, green).


(2015-09-18)  

 Leopold Gmelin  (1788-1853)  Ferroxyl indicator  is an aqueous solution containing red prussiate  (potassium ferricyanate),  with phenolphthalein  and sodium chloride. It turns blue  in the presence of ferrous ions  (Fe++) due to the formation of Prussian blue.

 Come back later, we're still working on this one...


(2015-08-15)  
Dehydration of sugar produces a steaming column of foamy carbon.

Sugars are calledcarbohydrates because theycan decompose into carbon, water and nothing else. (Experiment with sucrose, glucose, fructose, etc.)

A very strong dessicant like concentrated sulfuric acid is able to break downsugar molecules to extract the water and leave only pure carbon behind.

The reaction combines sugar dehydration and dilution of water in sulfuric acid,which are both strongly exothermic.  Some of the heat produced converts water to steam.


(2011-08-27)  
1 g of sodium polyacrylate  can hold  825 mL  of water.

 Come back later, we're still working on this one...


(2011-08-28)  
A mixture that's ignited by water.

The main reaction is:

NH4NO3  +  Zn   N2  +  ZnO  +  2 H2O

However, it is best ignited by the following reaction,catalyzed by  Cl  ions:

NH4NO3   N2O  +  2 H2O

That subsidiary reaction can be started with a drop of concentrated hydrochloric acid. Alternately, pure water (or just moisture) will ignite a mixture thatalready contains a little bit of chlorine ions, in the form ofammonium chloride  (or sodium chloride). Also, the acidity may remove the oxidation layerof zinc to make the metal available for the main event.


(2011-09-06)  
An explosive set off by the touch of a feather or by alpha radiation.

 Come back later, we're still working on this one...

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