Chemistry 100 Laboratory (1 Semester, Monthly Grading Period) Chemistry laboratory work place where discovery and learning

rning is facilitated Made to avoid the use of highly toxic, hazardous and carcinogenic substance from the experiment in this laboratory manual. SAFETY FIRST basic principle employed in chemistry laboratory Attire o Wear prescribed laboratory gowns and safety goggles must be worn at all times in the laboratory. This applies to everyone whether working or non working. o Contact lenses not allowed even when worn under safety goggle. Fumes may case serious injuries or blindness o Closed-toe shoes and long pants must be word in lab. Sandals and shorts are not allowed o Ladies = long hair must be tied back when doing experiments Conduct o Eating and drinking are PROHIBITED o Designated experiments are to be performed; Consult laboratory instructor if you have questions. o Never attempt to taste anything or put anything used in the experiment in your mouth. o Avoid smelling any vapor or gas unless procedure requires it. Waft a small sample to the nose using cupped hand o Bags and all belongings unnecessary for lab performance to be placed in bag rack. o Wash hands after handling chemicals and before leaving laboratory o Find safety and first air equipment (location) [fire extinguisher, showers and eye-wash stations] o Inform lab instructor incase of accident o Cameras and other electronic gadgets are allowed only if approved by the laboratory instructors Proper Handling of Chemicals and Equipment o Consider all chemicals to be hazardous unless instructed otherwise. Take note of the chemical precautions o Take note of chemicals and amount needed for experiment. Read label twice. If in doubt ask instructors first o Do not bring reagent bottles to working table. DO NOT DISARRANGE THEM o Use proper transferring apparatus for the reagent to avoid contamination o Always keep container covered if no one else will be taking from it anymore o Avoid getting excess reagents o Organic Solvents such as alcohols and acetone ARE HIGHLY FLAMMABL. DO NOT use them anywhere near open flames o Always pour acids into water. IF water is poured into acid, the heat of reaction will cause the water to explode into steam, sometimes violently and acid will splatter o If chemicals come into contact with skin or eyes, flush immediately with water and consult instructor o Never point a test tube or any vessel to anyone while heating o Dispose chemicals properly. Waste bottle specific for reagents used will be provided unless explicitly told, assume that only water may be discarded in the lab sinks. Solid wastes should be thrown on the trash can o Clean up and dispose all broken glassware. Use broom and dustpan for cleaning o Ask lab tech for assistance to clean up hazardous spills o Never leave burners unattended o Be sure gas and water valve shut off when leaving lab o Beware of hot glassware = looks like cold glassware o Always keep reagent and apparatus station clean o Check if working area clean, lockers locked, chairs arranged before leaving the laboratory o Do not leave the lab without the permission of lab instructor Most Common Hazard Symbols

st

EXPLOSIVE

OXIDIZING

FLAMMABLE

TOXIC

HARMFUL

IRRITANT

CORROSIVE

RADIOACTIVE

Appendix A o CATIONS : Positive Ions MONOVALENT (1+) NH4 Ammonium Cs Cesium Cu Copper (1) // Cuprous Au Gold (1) // Auric H Hydrogen Li Lithium K Potassium Ag Silver Na Sodium Divalent (2+) Ba Barium Be Beryllium Ca Calcium Cr Chromium (II) // Chromous Co Cobalt (II) // Cobaltous Cu Copper (II) // Cupric Fe Iron (II) // Ferrous

Pb Lead (II) // Plumbous Mg Magnesium Mn Manganese (II) // Manganous Hg2 Mercury (I) // Mercurous Hg Mercury (II) // Mercuric Ni Nickel (II) // Nickelous Sr Strontium Sn Tin (II) /// Stannous Zn Zinc Trivalent (3+) Al aluminum Cr Chromium (III) / Chromic Co Cobalt (III) / Cobaltic Fe - Iron (III) / Ferric Tetravalent (4+) Pb Lead (IV) // Plumbic Ni Nickel (IV) / Nickelic Sn Tin (IV) // Stannic

Anions Monovalent (1-) CH3COO Acetate NH2 Amide Br Bromide BrO3 Bromate BrO Hypobromite Cl Chloride ClO2 Chlorite ClO3 - Chlorate ClO4 Perchlorate ClO Hypochlorite CN Cyanide CNO Cyanate SCN Thiocynate H2PO4 Dihydrogen phosphate // Primary phosphate F Fluoride I Iodide H Hydride HCO3 Hydrogen carbonate/Bicarbonate HSO4 Hydrogen sulfate // bisulfate OH Hydoxide IO3 Iodate NO2 Nitrite NO3 Nitrate MnO4 Permanganate Divalent (2-) CO3 Carbonate O Oxide C2O4 Oxalate CrO4 Chromate O2 Peroxide HPO4 Hydrogen phosphate/biphosphate // Secondary phosphate S Sulfide SO3 Sulfite SO4 Sulfate S2O3 Thiosulfate S406 Tetrathionate Trivalent (3-) N Nitride AsO3 Arsenite AsO4 Arsenate PO4 Phosphate // Tertiary phosphate Appendix B o Naming Chemical Formula IUPAC (International Union of Pure and Applied Chemistry Devised a system for naming chemical compounds and writing chemical formula Rules for Naming Type Binary Compounds A binary compound is a chemical compound made up of two elements o Cation name + Anion A simple cation (obtained from a single atom or monoatomic) takes its name from the first name of the element. A simple anion (monoatomic) is named by taking the first part of the element name (root plus adding the letters ide

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Write name of compound by combining names of ions (Cations = capital letter; anions small letter) Stock System some cases for simple cations having several oxidation numbers, roman numeral is used to indicate oxidation number (charge) of the metal cation In case of gases prefixes are used to indicate number of atoms in chemical formula o Mono not used for naming first element Rules for Naming Ternary Compounds Polyatomic ion a group of atoms with an electric charge. o Nearly all polyatomic ions end with the letters ate or ite. (exceptions: cyanide (CN), hydroxide (OH), Peroxide (O2) ends with ide) -n -n -n -n -n X o XO o XO2 o XO3 o XO4 X-ide o (hypo-X-ite) o (X-ite) o (X-ate) o (per-X-ate) Chloride o hypochlorite chlorite o chlorate o perchlorate cyanide o hypocyanite o cyanite o cyanate o percyanate sulfide o o o sulfite o sulfate o In cases when polyatomic anions contain Hydrogen (H) at the beginning of the formula, bi is added to the name of the ion o Follow naming systems for binary compounds but do not change the name of polyatomic ions Rule for naming acids All acids begin with Hydrogen. Names of most acids end with the word acid. Two types of acids o Contain oxygen o Do not contain oxygen Hydochloric acid = HCL in aqueous form Hydrogen chloride or Hydrogen halide = HCL in gaseous form o Writing Chemical Formula Monoatomic ions Identify symbols of cation and anion. Write their symbol together with their respective valence charge. Cation is placed on left, anions on right Balance the positive and negative charge. Write the formula placing the subscripts right after the symbol they go with. The numbers inside parenthesis become the subscripts in the formula Understood if subscript 1 = none is written Subscripts not written if both ions have same value for oxidation number Polyatomic Ions Identify symbols of cation and anion. Write symbols together with respective valence charge. Treat polyatomic ion as single unit Balance positive and negative charges Write formula placing subscripts after the symbol they go with. Numbers inside parenthesis become subscripts in formula Appendix C o Numbers Exact numbers obtained in counting, does not need measuring tool to report quantity Measure numbers measuring tool is used to determine quantity, mass, length, volume of an object o Significant Figures in Measurement Measured numbers = all figures are called significant figures Non-zero digits are always significant Zeros between non-zero digits are significant (Sandwiched zeros) Zeros at end of a decimal are counted as significant (When a non zero digit is on its right side) Placeholders or leading zeros are not significant. Merely express magnitude of number (when zeros are on the right of the non zero digit) When a number is written in scientific notation, all figures in coeff are significant In measurement, last sig. fig is always the estimated digit When multiplying or dividing measured numbers: o Count number of sig fig in each expression which will be multiplied or divided o Report answer based on least number of significant figures of numbers multiplied or divided When adding or subtracting measured numbers, report answer has the same number of decimal places as the measure number with fewest decimal places Add&Subtract and Multiply&Divide rule does not apply to counting number (exact numbers) such as coeff, integers o Rounding Off If the number to be dropped is less than 5, the preceding number is retained and all following numbers are dropped. If first number to be dropped is 5 or greater, the numbers are dropped and the preceding digit is increased by 1. To avoid propagation of error, do not perform rounding off numbers in the middle of any computation

Appendix D (Common Laboratory Apparatus and Equipment) o Reservoir for Chemicals/Liquids Beaker Florence flask Erlenmeyer flask Reagent Bottle o For accurate volume measurement Pipette (volumetric and measuring) Burette (Geisler, Mohr, Universal) o For Mass measurement Triple beam balance Top loading balance Weighing bottle o For Mechanical support Tripod Iron stand Iron ring Crucible with cover Buret clamp (single or double) Iron clap Wire gauze Clay triangle Test tube holder Test tube rack Crucible tong o For transferring chemicals Funnel Dropper / Pasteur pipette Spatula (porcelain or stainless steel) Stirring rod o For Approximate Volume measurement Graduated cylinder Beaker Erlenmeyer flask o For Heating Bunsen Burner Hot plate Test tube Hard glass test tube Crucible with cover o For Distillation Distilling flask Condenser Thermometer Adapter o Miscellaneous Apparatus / Equipments Fumehood used to ventilate noxious or harmful gases Mortar and Pestle grind solid substances into powder form Spot plate used for qualitative analysis of small amount of chemicals/samples Volumetric flask for preparation of solution Watch glass for holding minute samples; for covering beaker or evaporating dish Evaporating dish used to evaporate solvent in mixture, leaving residue behind Test tube brush for cleaning test tube Desiccator used to provide low-humidity environment for chemicals/samples to prevent reabsorption of moisture; contains desiccant, a drying agent Wash bottle used to dispense small volumes of distilled water Appendix E (Basic Laboratory Techniques) o Heating Lab. Equipment: Bunsen Burner Source of heat; combustible gas (e.g. natural or liquefied gas) is mixed with correct amount of air to yield the maximum amount of heat. Princpal parts: o Needle valve quantity of combustible gas that enters the burner is regulated by this o Air holes flow of air needed for combustion is admitted through this o Barrel moving steam of gas and air are premixed in the barrel before it enters combustion zone at top of the burner Burner is connected to gas outlet by rubber/plastic tubing Size and quantity of flame generated = adjusted = by regulating amount of combustible gas or air Combustible gas = used to supply fuel for burner = mixture of hydrocarbons but composition is primarily methane (CH4) EQUIMOLAR AMOUNT OF AIR IS MIXED WITH GAS o Blue / non-luminous flame is generated

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COMPLETE COMBUSTION More heat! CH4(g) + O2(g) CO2(g) + 2H2O(l) Suitable for most lab purposes because it is hotter and doesnt stain glassware with soot.

INSUFFICIENT AIR o Luminous flame / Yellow o Yellow and smoky due to soot particles (unburned carbon/carbon monoxide soot particles) o INCOMPLETE COMBUSTION o Air holes are fully closed o Cooler! Air holes fully open o Too much air enters barrel causing burner to produce hissing sounds or flame to blow out (strike back) Basic Operation of Bunsen Burner Connect rubber tubing to the gas outlet Make sure that needle valve is closed. Close the air holes by adjusting the collar. Light a match at the open-end of the barrel. Then slowly open the gas outlet and needle valve to let gas enter the burner. A slight hissing sound could be heard as the gas escapes. Adjust gas outlet or needle valve till height of flame is about two inches tall. Adjust the collar found at the base of the barrel till a blue flame is produced. Turn off needle valve and or gas outlet to extinguish flame. IF STRIKE BACK HAPPENS, TURN OFF NEEDLE VALVE TO AVOID EXPLOSION. Do not leave opened burner unattended. Close burner if it is not being used. Basic Techniques in heating Heating using test tube o Transfer reagent that needs to be heated in a test tube. LIMIT. Fill test tube not more than half of its capacity o Do not hold test tube with bare hands. o Make sure that open end of test tube is pointed away from everyone at all times o DO NOT heat a test tube with a stopper, most especially if it contains chemicals that will release gases during heating. Pressure will build up and can cause ejection of the stopper or explosion which can lead to injury. o Heat gradually and slowly to prevent bumping. Hold test tube at 45* angle and pass tube back and forth over flame instead of holding it in one place Bumping sudden boiling of liquid forcing the liquid out the tube due to rapid heating Heating using water bath o Commonly used to heat flammable liquids or reagents that easily decompose when heated over direct flame o Substance placed in vessel (test tube/beaker) the would be immersed into larger vessel containing water which is kept at desired temperature. o Liquid/reagent can only be heated in water bath if its boiling point is less than that of water AVOID filling water bath with too much water. Might overflow when putting the vessels Level of water should be enough so that it is above level of the substance in tube Do not allow water to reach boiling point, might cause bumping which leads to water entering tubes. Mass Measurement Triple Beam Balance Sensitivity smallest weight that will produce a certain measureable response Readability smallest discernable scale division Most common lab equipment for mass measurement 0.1 g Smallest scale division and can be measured to as small as 0.05 g NEVER DIRECTLY WEIGH SOLID SUBSTANCE ON BALANCE PAN, CORROISION may occur. Parts of TB Balance o Pointer determine mass measured balance by riders o Scale series of lines along which pointer moves o Zero point center line of scale o Adjustment screw use to set balance at zero point when riders are all on zero o Pan platform where object being weight is placed o Beams horizontal structures with graduations that indicates mass in grams; as the name implies, it has three beams, each supporting different weights

o Riders weight move along beams used to balance object Basic operation o Make sure pan is empty and clean and all riders are set to zero o Adjust adjustment screw if pointer is not set to zero o Place the object on pan. The pointer goes above zero since it is not balanced. Move rider one notch at a time until pointer goes back to the zero mark If pointer goes down below zero, it means the total weight of the riders is more than the mass of the object. Readjust by moving it back. o Read mass of object. Its equal to the sum of the readings on the three beams If chemicals are being weight, put it inside any glassware such as weighing bottle or beaker to serve as container for chemicals to be weighed. o Measure mass of clean and empty container o Readjust riders so mass reading is sum of the mass of the container and chemicals o Transfer chemicals into empty beaker (on the pan) until pointer rests at zero mark Maintenance of Triple Beam Balance o Place on top of a stable counter table to avoid vibrations. Place in a room with minimal air fluctuations o Clean the pan after every use of the balance o Place back all riders at zero position. Make sure pointer rests at zero point o Never weigh hot objects! Allow to cool first. o Notify lab tech if balance is not working properly Volume Measurement To Deliver (TD-type) of glassware lab apparatus designed to deliver specified volume at the calibration temperature. (all are in mL) Used to approximately or accurately measure volume of liquids Reading Volume Meniscus shallow curve on surface of the liquid Bottom of the meniscus is the level of the solution. Eye should be same level as bottom of the meniscus to avoid parallax error Use of Pipette TD-type glassware used to accurately deliver single (volumetric pipette) or variable (measuring pipette) volumes of liquid 0 mark is found at the top part Volume is read after liquid has been dispensed. o Rinse w/ small amount of liquid to be transferred. Wet entire inside of surface by drawing liquid into tip and rotating pipette horizontally, discard rinsing o Draw in liquid with aspirator (Never use mouth to suction liquid) o Carefully fill pipette above zero mark. o Quickly replace aspirator with index finger. NO bubbles must be present o Touch tip of pipette on wall of vessel (other than the receiving vessel) then slowly allow liquid to drop until it reaches the graduation mark. (rotate using thumb and middle finger) o Touch tip on wall of vessel to remove drops clinging outside pipette o Place pipette within receiving vessel and allow liquid to drain freely. DO NOT force drain liquid o Blow-out pipette used = blow out drop of liquid adhering to tip using aspirator. IF NOT, then dont its not part of volume measurement o Immediately rinse pipette with distilled water after use. o PCR Press aspirator, connect aspirator to pipette, release slowly Use of Burette (Titration) Titration process of adding small amount of reagent of known concentration (contained in a burette) to a flask containing reactant until reaction is complete. Universal burette long highly uniformed diameter tube marked with volume graduations and fitted with Teflon stopcock. Commonly used in titration Technique in titration and proper usage of burette o To fill up burette with solution, make sure stopcock is closed. o Add small amt of solution to be transferred and then rotate burette horizontally to wet interior completely o Drain liquid through tip by opening stopcock. Once completely drained, close the stopcock. o Support burette within iron stand and burette clamp. Fill burette with solution above zero mark o Free tip from air bubbles by opening stopcock, permitting solution to pass through tip. Once tip is filled with solution. Immediately close stopcock. o If level of solution is above zero mark, adjust by draining some of solution out of burette. If solution is below zero mark, add more using a dropper. Note the initial volume reading.

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Place tip of burette within titration vessel (Erlenmeyer flask) Deliver small amount of solution by slowly opening stopcock Swirl vessel constantly to ensure completeness in reaction between reactants Add solution drop-wise when endpoint is near. Can be observed when development of persistent color. (White background for easy visualization of end point) If reaction is judged to be complete close stopcock and then take note of final volume reading. Volume of solution delivered into vessel is the difference between final and initial volume reading.

Preparation of Solutions Volumetric flask glassware used for dilution and preparation of solutions. Pear shaped, flat bottomed flask with a long, narrow neck that has an etched graduation mark. TC-type of glassware (To Contain) it will only contain and not deliver a specified volume of liquid at a particular temperature. How to prepare solution? A weighed solid reagent is dissolved in a beaker with a minimum volume of solvent (usually water) The solution is transferred into volumetric flask using stirring rod to direct flow. Rinse both stirring rod and beaker with distilled water and transfer washings to volumetric flask. Repeat this step at least two more times Half fill the flask with solvent and swirl the contents. Add more solvent until level of liquid almost reaches mark Use dropped for final additions of solvent, bottom meniscus should be same level as graduation mark Cover flask with stopper, invert it several times to make homogenous solution. Transfer contents in storage bottle. o Rinse reagent bottle with small amount of prepared solution. Discard rinsing. Transfer solution into bottle Label bottle EXPERIMENT 1: NUMBERS AND MEASUREMENT o Measurement quantitative expression of observed physical property of matter; derived from GREEK work metron meaning limited proportion o Metric system system of measurement used in science, industry and medicine; also called DECIMAL SYSTEM (measurements of each type are related by factors of 10) length - meter o English System uses many units of length such as inch, foot, yard, mile o Unit always be included when reporting a measurement; required to complete measurement reported o Kilo larger quantities; milli smaller quantities o SI Base Units (International System of Units SI base units for seven base quantities, which were assumed to be mutually independent. o SI Derived Units Derived units defined accd. to seven base units through a system of quantity relationships o Conversion of Unit of Measurement Take note of units to be converted Determine common conversion factor for these units Multiply factor with given measure to be converted Be sure factors are arranged in such a way that units of the given unit will cancel out. Perform operation to determine the converted measurement The procedure above does not apply to temperature. Follow a diff. conversion method F* - C* = C= (F-32)(5/9) C* - F* = *F = (9/5)*C+32 *C K = K = *C + 273.15 o Accuracy VS. Precision Accuracy Precision Accuracy is how close a measured value is to Precision is how close the measure values are the actual (true) value. to each other. May be determined by single measurement It may be determined through several measurements Measurements are very close to the standard, true or known values. Measure of reliability and reproducibility the experiment The farther a measurement is from its expected value, the less accurate it is. If such observations are closely clustered together, then, these observations are considered to have been obtained with high precision. No perfect measurement Accurate but not precise/ precise but not accurate/ neither or both PERCENTAGE ERROR o % error = (True value Experimental value) / true value X 100

COEFFICIENT OF VARIATION o Coeff of variation = Standard Deviation / mean X 100 2 o Where standard deviation = (x-mean) / n-1 o X = score; n = number of data