CHAPTER 3 APPARATUS, TECHNIQUE AND REAGENTS TYPES, CARE AND USAGE OF ANALYTICAL BALANCES Analytical Balance used to measure

sure mass Have 3 types:-

1. Electronic analytical balance Typical properties : 1. Capacity to weigh 100 200 g 2. Measure to nearest 0.01 to 0.001g

2. Mechanical analytical balance 2 types :1. Single pan (unequal arm) 2. Equal arm

3. Auxillary balance eg. Top pan balance

Care Of Analytical Balance 1. The balance should not be placed near an open window or directly in front of the air-condition air vent. This will cause draft. 2. The balance should have a stable support usually a concrete bench. 3. The balance should not be place where there is direct sunlight. 4. The room should be air-condition 5. Always handle with great care. Never drop the analytical balance. Usage Of Analytical Balance Weighing of solids Direct weighing. 1. A weighing dish/bottle/boat is used. 2. The dish or boat is weighed empty and then with the sample. 3. Direct weighing is satisfactory only if the sample is nonhygroscopic. Weighing of liquids/solution 1. The liquid is transferred to a weighing vessel (eg. a weighing bottle) which is capped to prevent evaporation during the weighing, and is then weighed.

Weighing by difference 1. Solid chemical materials are usually weighed and dried in a weighing bottle. 2. Replicate weighing are most conveniently carried out by weighing by difference. 3. Also if the sample is hygroscopic, weighing by difference with the bottle capped must be employed.

 TYPES, CARE AND USAGE OF PIPETTE, BURETTE AND VOLUMETRIC FLASK

Pipettes Used to transfer a particular volume of solution. Permit the transfer of accurate known volume from one container to another Used to deliver a certain fraction or portion of a solution

Two Common Types Of Pipets : Volumetric or transfer pipet (TD) - used for accurate measurements since it is designed to deliver only one volume and is calibrated at that volume. Volumetric pipets are available in sizes of 100 mL to 0.5 mL or less Measuring or graduated pipette. (clinical, Mohr or serological pipette) - Measuring pipetsare straight bore pipetes that are marked at different volume intervals. Therefore these pipette is TC. These pipettes are not as accurate as bulb pipette due to non-uniformity of the internal diameter of the device . It will have a relative larger error effect on total volume then is the case for pipettes with a bulb shape. The measuring pipettes range from a total volume of 25 to 0.1 mL.

Techniques For Using A Pipette 1. Clean the pipette with detergent and water. 2. Rinse the pipette thoroughly, first with tap water and then with distilled water. 3. Rinse the pipette twice with a small volume of the solution to be transferred 4. Using a filler (such as rubber pipette bulb, pipette pump) fill the pipette above the calibration mark. 5. Hold the pipette vertically with the tip against a beaker. 6. Use a tissue paper to remove drops on the outside of the pipette near the tip. 7. Mark at eye level allow the solution to drain slowly until the bottom of he meniscus is level with the calibration. If the bottom of the meniscus falls below the calibration, start again to refill using the safety filler. 8. Allow the content to drain into the conical flask freely. Hold the pipette tip against the flask wall to avoid splashing. 9. After the pipette appears to have drained, allow five seconds further drainage. Do not force the contents out of the pipet. 10. Wash down the inside walls of the flask with distilled water from a wash bottle. 11. No solution should be pipetted by mouth.

 Burette used for the accurate delivery of a variable amount of solution. Its principle use is in titration, where a standard solution is added to the sample solution until the end point is reached. The conventional burette for macrotitration is marked in 0.1 mL increments from 0 to 50 mL. The volume delivered can be read to the nearest 0.01 mL by interpolation. Techniques For Using A Burette 1. Clean the burette with detergent and water and rinse it with distilled water. 2. Rinse the burette twice with 5-10 mL portions of the solution to be transferred. 3. Using a small funnel, nearly fill the burette with the solution to be transferred. 4. Remove the funnel. 5. Open the tap to run out the bubble in the burette tip (or lightly knock on the glass tip) and allow the meniscus to fall to a level between 0 and 5 mL calibrations 6. Touch a beaker against the tip to remove any drop that has not fallen off. 7. With the burette vertical and the meniscus at eye level, estimate to the nearest 0.02 mL the level of the bottom of the meniscus. Record this initial reading 8. Transfer solution from the burette into the receiving conical flask until the end point is reached. 9. Use your right hand to swirl the conical flask. 10. Record your final reading. The difference between your initial and final reading is the titre (titer) (ie. the volume of liquid delivered from the burette)

Volumetric Flask 1. Used in the diluting of a sample or solution to a certain volume. 2. The volumetric flasks come in a variety of sizes, ranging from 1.0 mL or more to 2.0 L. 3. The flask are designed to contain an accurate volume at the specified temperature (20 or 25oC). 4. These flasks are marked with TC to indicate to contain.

Types Of Volumetric Flask

Grade A tolerances are approximately halved that of Grade B. Grade A flasks come with a certificate of calibration (more accurate). Care And Usage Of Volumetric Flask 1. Initially, a small amount of diluent (usually distilled water ) is added to the empty flask. 2. Reagent chemicals should never be added directly to a dry flask surface, as glass is highly absorbent to concentrated substances. 3. Then the desired chemical reagent (either solid or liquid) is added to the flask. 4. Then the diluent (dilution solvent) is added to fill flask about 2/3 and flask is swirl to mix mixture before diluent is further added to the neck of the flask. 5. Finally diluent is added to the meniscus carefully in dropwise manner. 6. The solution is finally thoroughly mix by inverting the flask and swirl or shake vigorously for 10 sec. Turn right side-up and repeat the invertion, shaking or swirling for at least 10 times.

TECHNIQUE TO CALIBRATE THE VOLUMTERIC GLASSWARE There are three general methods commonly employed to calibrate glassware. These are as follows: 1. Direct, absolute calibration 2. Indirect, absolute calibration 3. Relative calibration

Direct calibration: A volume of water delivered by a burette or pipette, or contained in a volumetric flask, is obtained directly from the weight of the water and its density. Indirect calibration: Volumetric glassware calibrated by comparison of the mass of water it contains or delivers at a particular temperature with that of another vessel which had been calibrated directly. The volumes are directly related to the masses of water. This method is convenient if many pieces of glassware are to be calibrated. Relative calibration: volumetric relationship between two items of glassware without knowing the absolute volume of either. This situation arises, for example, in taking an aliquot portion of a solution.

Calibration of a 50 ml volumetric pipette

1. Ensure the pipet you desire to calibrate is clean. If small droplets of water adhere to the inner surface of the pipette after delivering deionized water, the pipette is dirty and must be cleaned before proceeding further. 2. Determine the mass of the empty, stoppered receiver to the nearest milligram. 3. Transfer the 50 mL volume from pipette into a stoppered container. 4. Weigh the stoppered receiver and its contents and calculate the mass of water delivered by difference. 5. From the delivered mass of water, calculate the volume delivered using the appropriate density data table. 6. Repeat the calibration three times and calculate the mean volume delivered and the standard deviation.

TYPES, USAGE AND TECHNIQUE USING BURNERS, HOTPLATES, OVENS, FURNACE AND WATER BATH

Burners - Used when heating a substance in a beaker or crucible, supported on a ringstand by means of a wire gauze or clay triangle.

BARREL is the area where the air and gas mix COLLAR can be turned to adjust the intake of air GAS INTAKE TUBE brings the supply of gas from the outlet to the burner SPUD is the small opening through which the gas flows.

Technique 1. Join the burner to a gas tap 2. Close the air hole 3. Light a match and hold it over the chimney. Turn on the gas tap. 4. To make the flame burn hotter and larger, open the air mixture valve accordingly and will produce blue colour of flame. 5. To make the flame burn cooler and smaller, close the air mixture valve accordingly and will produce yellow colour of flame. Usage 1. Remove all flammable and combustible materials from the lab bench and surrounding area when the bunsen burner is used. DO NOT use a bunsen burner when working with flammable liquids or solvents. 2. Always check for any gas leak to prevent sudden explosion when lighting up the bunsen burner 3. To light up a bunsen burner, close or partially close a bunsen burner to make it easier to light

Hot Plate - Used for speedy heating up of any solutions in a container or under controlled temperature

Usage and Technique 1. Always wear safety glasses or other safety equipment while operating the equipment 2. Do not immense the hot plates while cleaning 3. Do not heat or stir volatile materials 4. Do not use foil, metal container and heavy glassware container 5. Use only heat resistant brosilicate glassware 6. Turn off the hot plates when not in use

Ovens Two types of ovens : a) Electric Oven Usage and Technique 1. Laboratories for drying sample or products. 2. Growing field of medical, agricultural, industrial research for day to day heating, 3. Drying, sterilizing, baking etc. 4. Getting rid of fungus by application of dry heat 5. Wear heat resistant gloves 6. Do not put hazardous object into the oven 7. Use safety glass or shield b) Microwave oven Usage and Technique 1. Microwave oven are designed to cook food. 2. Not to do scientific experiment. 3. In the lab, it is used for digestion of samples during sample preparation. 4. Wear heat resistant gloves 5. Do not put hazardous object into the oven 6. Use safety glass or shield

 Electric Furnace 1. It is use in a fabricant facilities as it is use to form gate oxides and dope materials to be chemically active. 2. It is easily poisoned by impurities. 3. Impurities dissolved in glass and ruin the sample after initial contamination. Types of furnace Oxidation - This is the cleanest furnace and can only be used to oxidized. Phosphorus doping - used to dope selected materials N-type conductor. Boron doping - used to dope selected materials P-type conductor. General annealing - relatively dirty since a large variety of samples will go through it.

Usage and Technique 1. Never put anything that has not been thoroughly cleaned into the furnace. 2. Never exchange parts of one furnace to put in another. 3. Never touched the furnace with your bare hands.

Water Bath Usage Of Water Bath 1. used to heat those substances, which can't be heated directly on Bunsen burner or hot plate or any other such media. 2. only those materials can be heated with water bath whose boiling point is less than that of water. 3. used in a variety of applications such as in industrial clinical laboratories, academic facilities, research laboratories, environmental applications Technique Using Water Baths 1. Set the maximum temperature the waterbath should attain. 2. Avoid to touch the inner of the waterbath while it is hot. 3. Use air jacket heating to avoid hot spots.

 USAGE AND CARE OF DESICCATORS 1. Desiccators made from heavy moulded brosilicate glass. 2. Desiccator are sealable enclosures containing desiccants used for preserving moisture sensitive items 3. Also used to remove traces of water from an already dry sample 4. It used to keep samples dry while cooling and before they are weighed and to dry wet sample. 5. Dried or ignites samples and vessels are cooled in the desiccator. 6. A porcelain plate is usually placed in the desiccators to support weighing bottles, crucible, and other vessels. 7. An airtight seal is made by application of stopcock grease to the groun-glass rim on the top of the desiccator. 8. A vacuum desiccator has a side arm on the top for evacuation so that the contents can be kept in a vacuum rather than just an atmosphere of dry air. 9. Dont move the top of desiccator since the removal of moisture from the air is rather slow. 10. A red-hot crucible or other vessels should be placed in air to cool before place in desiccator.

 FILTRATION APPARATUS AND TECHNIQUE

Filtration is a technique used for two main purposes:1) The first is to remove solid impurities from a liquid. 2) The second is to collect a desired solid from the solution from which it was precipitated or crystallized. Several different kinds of filtration are commonly used: two general methods include gravity filtration and vacuum (or suction) filtration.

Filtration Apparatus Apparatus Gravity Filtration Filter cones The volume of liquid to be filtered is about 10 mL or greater, and the solid collected in the filter is saved. The volume of liquid to be filtered is greater than 10 mL, and solid impurities are removed from a solution; often used in crystallization procedures. Used with small volumes, less than about 10 mL, to remove solid impurities from a liquid. Vacuum filtration Hirsch funnels Primarily used to collect a desired solid from a relatively small volume of liquid (1-10 mL); used frequently to collect the crystals obtained from crystallizations. Used in the same way as Hirsch funnels, except the volume of liquid is usually greater. Used to remove finely divided impurities. Application

Fluted Filters

Filtering pipets

Buchner funnels Filtering Media

Gravity Filtration: This method uses gravity to reach the goal of separation through filtration. The most familiar technique is probably filtration of a solution through a paper filter held in a funnel, allowing gravity to draw the liquid through the paper. Because even a small piece of filter paper will absorb a significant volume of liquid, in most microscale procedure requiring filtration, this technique is useful only when the volume of mixture to be filtered is greater than 10 mL. For many microscale procedures a more suitable technique, which also makes use of gravity, is to use a Pasteur (or disposable) pipet with a cotton or glass wool plug (called a filtering pipet).

Filtration Technique

Gravity Filtration:Filter cones: This filtration technique is most useful when the solid material being filtered from a mixture is to be collected and used later. The filter cone is likely to be used in a microscale experiments only when a relatively large volume (greater than 10 mL) is being filtered and when a Hirsch funnel is not appropriate.

How to set up a gravity filtration? 1. Prepare a filter cone:

2. Gravity filtration with a filter cone:

With filtrations using a simple filter cone, the solvent may form a seal between the filter and the funnel and between the funnel and the lip of the receiving flask. When a seal forms, the filtration stops because the displaced air has no possibility of escaping. To avoid the solvent seal, you can insert a small piece of paper, a paper clip, or some other bent wire between the funnel and the lip of the flask to let the displaced air escape.

Fluted filters: Fluted filters are also most useful when filtering a relatively large amount of liquid. They are often used to filter a hot solution saturated with a solute during a crystallization procedure. The major advantage of a fluted filter is that it increases the speed of filtration for two reasons: first, it increases the surface area of the filter paper through which the solvent seeps; second, it allows air to enter the flask along its sides to permit rapid pressure equalization.

How do I to use a fluted filter? 1. Prepare a fluted cone. Following are separate steps:-

2. When doing hot filtration, it is important to ensure that the filter does not become clogged by solid material accumulated in the stem of the funnel or in the filter paper. When the hot saturated solution comes in contact with a relatively cold funnel, the solution is cooled and may become supersaturated. If crystallization occurs in the filter, either the crystals will clog the filter paper or they will clog the stem of the funnel.

Four ways to keep the filter from clogging:

Use a short-stemmed or a stemless funnel; Keep the liquid to be filtered at or near its boiling point at all times; Preheat the funnel by pouring hot solvent through it before the actual filtration; Keep the filtrate (filtered solution) in the receiver hot enough to continue boiling slightly.

Vacuum (or suction) Filtration:

Vacuum, or suction, filtration is more rapid than gravity filtration and is most often used to collect solid products resulting from precipitation or crystallization. This technique is used primarily when the volume of liquid being filtered is more than 1-2 mL. In a vacuum filtration, a receiver flask with a sidearm, a filter flask, is used. The sidearm is connected by heavy-walled rubber tubing to a source of vacuum. Thinwalled tubing (such as the tygon tube you use to connect cooling water) will collapse under vacuum, due to atmospheric pressure on its outside walls, and will seal the vacuum source from the flask.

 Filtration Technique

To perform a vacuum filtration, clamp the flask securely to a ring stand.

Add a Buchner funnel with a rubber funnel adaptor.

Obtain a piece of filter paper in the funnel that is small enough to remain flat but large enough to cover all of the holes in the filter. If necessary, you can cut a larger piece of filter paper down to size.

Place the paper in the funnel.

Connect the side arm flask to a vacuum source. Always use thick-walled tubing, since Tygon tubing will collapse under reduced pressure.

Wet the paper with a small amount of the solvent to be used in the filtration. This causes the paper to adhere to the plate and keeps materials from passing under the paper during filtration. Turn on the vacuum source. Make sure that the paper is secure on the filter, that air is being drawn through the paper, and that all of your apparatus is securely clamped.

Pour the mixture to be filtered onto the filter paper. The vacuum should rapidly pull the liquid through the funnel. Watch that particulates do not creep under the edges of the paper. If this happens, start over and carefully pour portions of the solution onto the very center of the paper.

Rinse the cake with a small amount of fresh, cold solvent to help remove impurities that were dissolved in the filtrate.

Carefully disconnect the rubber tubing.

Remove the filter paper and the collected solid that is on it.

Usually you will need to set the product on a watch glass and let it air dry for a while.

TITRATION APPARATUS AND TECHNIQUE Titration

A titration is a method of analysis that will allow you to determine the precise endpoint of a reaction and therefore the precise quantity of reactant in the titration flask. A buret is used to deliver the second reactant to the flask and an indicator or pH Meter is used to detect the endpoint of the reaction.

Doing a Titration

Begin by preparing your buret.Your buret should be conditioned and filled with titrant solution. You should check for air bubbles and leaks, before proceding with the titration.

Take an initial volume reading and record it in your notebook. Before beginning a titration, you should always calculate the expected endpoint volume.

Prepare the solution to be analyzed by placing it in a clean Erlenmeyer flask or beaker. If your sample is a solid, make sure it is completely dissoloved. Put a magnetic stirrer in the flask and add indicator.

Use the buret to deliver a stream of titrant to within a couple of mL of your expected endpoint. You will see the indicator change color when the titrant hits the solution in the flask, but the color change disappears upon stirring.

Approach the endpoint more slowly and watch the color of your flask carefully. Use a wash bottle to rinse the sides of the flask and the tip of the buret, to be sure all titrant is mixed in the flask.

As you approach the endpoint, you may need to add a partial drop of titrant. You can do this with a rapid spin of a teflon stopcock or by partially opening the stopcock and rinsing the partial drop into the flask with a wash bottle. Ask your TA to demonstrate these techniques for you, in the lab.

Make sure you know what the endpoint should look like. For phenolphthalein, the endpoint is the first permanent pale pink. The pale pink fades in 10 to 20 minutes.

If you think you might have reached the endpoint, you can record the volume reading and add another partial drop. Sometimes it is easier to tell when you have gone past the endpoint.

When you have reached the endpoint, read the final volume in the buret and record it in your notebook.

Subtract the initial volume to determine the amount of titrant delivered. Use this, the concentration of the titrant, and the stoichiometry of the titration reaction to calculate the number of moles of reactant in your analyte solution.

TYPES OF REAGENT BASE ON ITS PURITY AND USAGE Purity of reagents has an important effect on the accuracy of the chemical analysis

Classifying Reagent 1) Reagent Grade (GR) - Conform to the minimum standard set by the reagent Chemical Committee of the American Chemical Society that can be used in analytical work (ACS) 2) Primary Standard Grade (AnalaR): - It should have purity of 99.95% pure - The primary standard reagents have been carefully analyzed by supplier and the assay is printed on the container label (or provided). - Symbolized AR Analytical grade 3) Special-Purpose Reagent Chemicals:- Prepared for specific application - Examples- spectroscopic solvents and HPLC solvents.

Rules For Handling Reagents And Solutions 1. Select the best suitable grade of chemicals available for analytical work. Pick the smallest bottle to supply the desired quantity (prevent wastage and overdue. 2. Replace the cap of the reagent bottle immediately after use. 3. Hold the stopper of the reagents bottles between your fingers; never set a stopper on the table. 4. Never return any excess reagents to a bottle.

CLEANING SOLUTIONS PROCESS

Cleaning Of Glassware 1. Clean glassware is imperative for accurate and precise volumetric applications. 2. It is therefore necessary to thoroughly clean all glassware before use.

1. Using Warm Detergent A brief soaking in a warm detergent solution (Teepol) is usually sufficient to remove the grease and dirt responsible for water breaks. If detergent is ineffective, treatment with cleaning solution usually helps. Films which adhere to the inside of flasks and bottles may often be removed by wetting the surface with dilute nitric acid, followed by multiple rinses with distilled water. 2. Concentrated Acid Concentrated HCl dissolves many metals and many metallic oxides Hot concentrated nitric acid dissolves most metals Films which adhere to the inside of flasks and bottles may often be removed by wetting the surface with dilute nitric acid, followed by multiple rinses with distilled water. Hot concentrated sulfuric acid dissolves many substances, many organic materials are charred and oxidized

3. Potassium Dichromate Sulfuric Acid Cleaning Solution This solution must be prepared and handled with extreme care. Eye protection must be worn at all times during use and avoid contact with clothing and skin. To prepare dissolve 92 g sodium dichromate in 458 mL water and cautiously add with stirring 800 mL concentrated sulfuric acid After the glassware has been cleaned with a detergent and rinsed carefully, pour a small quantity of the chromate solution into the glassware, allowing it to flow down all parts of the glass surface. Pour the solution back into its stock bottle. Rinse the glassware well. The cleaning solution may be reused until it acquires the green color of the chromium (III) ion. Once this happens, it should be discarded. Chromate cannot be disposed of in community waste water system

4. Aqua Regia Cleaning Solution Aqua Regia must be prepared and handled with extreme care. Wear eye protection at all times during use and avoid contact with clothing or skin Aqua Reqia is made up of three parts of concentrated HCl (75 vol%) and one part of concentrated HNO3 (25 vol%). Due to its oxidizing character, this is a very powerful and extremely dangerous and corrosive cleaning solution. Use in a fumehood with extreme care.

5. Ultrasonic Cleaning. Ultrasonic glass cleaners are very good for cleaning pipettes such as autopipette tips and buretttes. The glassware is soaked in a warm detergent solution through which is passed acoustic energy of frequency at or above 40 kHz. The ultrasonic vibrations dislodge dirt and grease quickly from the glass surfaces in most cases in a matter of 5 to 10 minutes.