SAINT MARY’S UNIVERSITY Bayombong, Nueva Vizcaya, Philippines SCHOOL OF HEALTH AND NATURAL SCIENCES CENTER FOR NATURAL SCIENCES Activity 1 INTRODUCTION TO THE ANALYTICAL BALANCE AND DESICCATOR INTRODUCTION The ability to determine mass accurately is fundamental not only to analytical chemistry but also to all of modern science. Practically speaking, all measurements which we shall perform in this course relate either directly or indirectly to a weighing using the single pan analytical balance. This is a delicate and precise instrument which, if kept scrupulously clean and handled correctly, will continue to yield reliable data during the course of its usage. It is therefore imperative that you become rapidly acquainted with your balance and that you gain assurance as to the correctness of your equipment and technique before proceeding with other experiments. Oven drying is the most common way of removing moisture from solids. This approach is not appropriate for substances that decompose or for those from which water is not removed at the temperature of the oven. The desiccator is used to store dried samples in a dry atmosphere. It should not be used to dry an object, but to maintain an already dried object indefinitely in a dry condition. To minimize the uptake of moisture, dried materials are stored in desiccators while they cool. OBJECTIVE This activity should enable you to accurately determine the mass of a sample using an analytical balance and demonstrate proper use of the desiccator PRE-LABORATORY Answer or explain substantially what is asked. Cite your references. 1. Define mass. Mass, denoted using m or M, is a dimensionless quantity representing the amount of matter in a particle or object (Tech Target Contributor, n.d.). Basically, it is a measure of the amount of matter in a substance or an object. The basic SI unit (International System of Units) or metric system for mass is kilogram (kg); smaller masses may be measured in grams (g). 2. What is the best tool to get mass? In determining an object's (substance's) mass, a balance, specifically analytical balance, is the best tool to be used. Analytical balance is a highly precise and/or accurate laboratory balance for measuring masses. Copyright 2021. All rights reserved. No parts of this document may be reproduced in any form or by any electronic means, including information storage and retrieval systems, without permission in writing from the author, except by reviewers, who may quote brief passages in a review. SAINT MARY’S UNIVERSITY Bayombong, Nueva Vizcaya, Philippines SCHOOL OF HEALTH AND NATURAL SCIENCES Typically, it FOR is designed with an enclosed measuring pan to avoid the CENTER NATURAL SCIENCES influences of dust and air currents, and may include vibration resistance, data transfer, automation, and capacity range options (Sartorius, n.d.). 3. Why is mass an important unit of measure in Chemistry? Mass is important to measure because it will measure the amount of force it will take to move the object. Mass is often measured by measuring an unmeasured object with standardized forms of measurements such as milligrams, grams and kilograms. 4. How can you assure accuracy in getting the mass? In order to protect the balance and ensure accurate results, the following ways should be properly observed: Always check that the balance is level before using; Do not weigh hot or cold objects; Clean up any spills around the balance immediately; and Never add chemicals or any unnecessary substances to a container. Additionally, according to Huntress (2021), the following steps are essential and practical to further ensure the precision and accuracy of mass (and other laboratory results/data): Keep everything calibrated. Calibration involves adjusting or standardizing equipment in the laboratory. Conduct routine maintenance. All lab instruments are needed to be given regular care to operate at their maximum. Operate in the appropriate range with correct parameters. Use tools that are designed and calibrated to work in the range you are measuring. Once unsure of measurements, reach out to any trusted peer or mentor for advice. Understand significant figures and record correctly. Keep significant figures consistent when measuring items repeatedly, and ensure the number of the same is appropriate for each measurement. Take multiple measurements. Detect shifts over time. Address the measurement drift issue immediately by recalibration or preventative maintenance. Consider “human factor”. Ensure that procedures are kept up to date, and that all lab personnel are properly-trained. Perform a measurement systems analysis). It mathematically determines the amount of variation that exists when taking measurements multiple times. MATERIALS AND REAGENTS Analytical Balance Desiccator Crucible Tongs Crucibles with cover Copyright 2021. All rights reserved. No parts of this document may be reproduced in any form or by any electronic means, including information storage and retrieval systems, without permission in writing from the author, except by reviewers, who may quote brief passages in a review. SAINT MARY’S UNIVERSITY Bayombong, Nueva Vizcaya, Philippines SCHOOL OF HEALTH AND NATURAL SCIENCES Weighing bottleFOR NATURAL SCIENCES CENTER Beaker Salt Procedures A. General Guidelines for Using the Analytical Balance 1. Chemicals are never placed directly on the weighing pan. A weighing boat, paper or bottle is used under the chemical. 2. Do not exceed the maximum weight limit of the balance. 3. Center the load on the pan as much as possible. 4. All objects or samples to be weighed must be in thermal equilibrium with the room before a weighing can be attempted. Temperature gradients within the balance case can result in convection currents, and the resultant draft against the pan will lead to erroneous weighing. 5. Never handle the item to be weighed directly with your fingers. 6. Immediately clean any chemical spillage on the pan, within the weighing chamber, or in the work area surrounding the balance. 7. Always record weights to the nearest 0.0001 g. Copyright 2021. All rights reserved. No parts of this document may be reproduced in any form or by any electronic means, including information storage and retrieval systems, without permission in writing from the author, except by reviewers, who may quote brief passages in a review. SAINT MARY’S UNIVERSITY Bayombong, Nueva Vizcaya, Philippines SCHOOL OF HEALTH AND NATURAL SCIENCES 8. CENTER Leave the sliding glass doors closed, the balance covered and the FOR NATURAL SCIENCES area around it clean. 9. Attend a demonstration by your instructor on how to operate the balance, and how to handle objects for weighing. B. Determining the Mass of an Object 1. Obtain a known sample from your lab instructor and record the sample identification number. Your sample contains five pellets of one color and ten of another. 2. Weigh each to 0.1 mg, recording your data in your laboratory notebook. Do not touch them with your fingers, as skin oils may change the mass of the pellets. Use tweezers or lintless paper or weighing paper to handle the pellets. 3. Reweigh the known sample 4 times. C. Weighing Out a Dispersible Sample The simplest and most effective method of weighing out samples is by difference. One approach is to first find the total weight of your sample container and its contents, pour or shake some of this material out into a labelled beaker or flask and finally reweighing the sample bottle plus remaining material. The difference between the initial and final weighing represents the sample mass. An alternative approach is to weigh the empty container, add the sample to the container, record its mass, and then quantitatively transfer its contents to a flask or beaker. The mass of the sample is the difference between the weight of the container plus contents minus the weight of the container. The object of this section will be to compare these two approaches. 1. Fill your clean, dry weighing bottle about 1/8 full with reagent grade NaCl. Be careful not to get material on the stopper. 2. Weigh the weighing bottle with NaCl to the nearest 0.1 mg. 3. Weigh a clean, dry 50 mL beaker to the nearest 0.1 mg. into the beaker on the balance pan, deliver 0.50 ± 0.01 g to the nearest 0.1 mg. of the NaCl from the weighing bottle. Record the final weight of the beaker. 4. Weigh the weighing bottle with residual sample. Compare the mass of NaCl added to the beaker with the mass of NaCl removed from the weighing bottle. 5. Weigh a clean, dry and empty weighing bottle. 6. Into the weighing bottle on the balance pan, deliver 0.250 ± 0.005 g to the nearest 0.1 mg. of the NaCl. 7. Record the final weight of the beaker. In the event that you spill NaCl onto the balance pan, arrest the balance, clean the pan and then repeat steps 6 and 7 D. Using the Desiccator 1. To open - slide lid horizontally across the top to one side until it comes off. Use one hand to hold the bottom of the desiccator while using the other hand to grasp the knob. Copyright 2021. All rights reserved. No parts of this document may be reproduced in any form or by any electronic means, including information storage and retrieval systems, without permission in writing from the author, except by reviewers, who may quote brief passages in a review. SAINT MARY’S UNIVERSITY Bayombong, Nueva Vizcaya, Philippines SCHOOL OF HEALTH AND NATURAL SCIENCES 2. To close - place lidNATURAL partly onSCIENCES the top and slide across until desiccator is CENTER FOR completely closed and then rotate lid gently in both directions. 3. Do not attempt to lift lid off vertically. 4. Make sure the lid has enough grease around the ground glass rim - if necessary, spread Vaseline uniformly on the rim. When the lid is improperly seated, the greased rim will appear as shown in Figure 3. On the other hand, when the lid is properly seated, the greased rim will appear. 5. If the desiccant appears wet or clumpy, it probably needs to be replaced with new desiccant. It is helpful to have a small amount of indicating desiccant present. When the color changes to pink, the desiccant should be replaced. 6. Desiccants should be handled in the hood and added carefully. Desiccant should not coat the sides or plate of the desiccator. 7. When placing a heated object in a desiccator, allow some cooling to occur before the lid is seated. 8. Transfer to and from the desiccator should normally not be by fingers but by crucible tongs or by strips of lintless paper. 9. It is also helpful to break the seal once or twice during cooling to relieve any excessive vacuum that develops. 10. Finally, lock the lid in place with your thumbs while moving the desiccator from one place to another. DATA AND RESULT 1. Draw or print and label the parts of an analytical balance and desiccator. Copyright 2021. All rights reserved. No parts of this document may be reproduced in any form or by any electronic means, including information storage and retrieval systems, without permission in writing from the author, except by reviewers, who may quote brief passages in a review. SAINT MARY’S UNIVERSITY Bayombong, Nueva Vizcaya, Philippines SCHOOL OF HEALTH AND NATURAL SCIENCES CENTER FOR NATURAL SCIENCES 2. Demonstrate how to properly use the desiccator To open the desiccator, slide the lid gently as shown at left. If you feel or hear metal scraping against metal when you slide off the lid, then a small amount of silicon grease needs to be rubbed around the flat surface of the lid. Squeeze quite small amount of grease onto your finger, as at the right, and rub it all around the flat surface of the lid. The desiccator contains a plate with holes over a screen which covers granulated anhydrous calcium sulphate, a desiccating or dehydrating agent. The desiccator ought not to be left open except to transfer samples in or out of it. (Hills, 2022) The following are the steps or key concepts to remember in properly utilizing a desiccator: Slide the cover horizontally with a gentle force until it starts moving. Grasp the knob with one hand, and with the other hold the base and apply more force to take it off completely; Do not get tempted to lift the desiccator by lifting the top knob. Always lift with both hands holding the bottom and the cover; Copyright 2021. All rights reserved. No parts of this document may be reproduced in any form or by any electronic means, including information storage and retrieval systems, without permission in writing from the author, except by reviewers, who may quote brief passages in a review. SAINT MARY’S UNIVERSITY Bayombong, Nueva Vizcaya, Philippines SCHOOL OF HEALTH AND NATURAL SCIENCES To close, lid gently on top and close slowly by applying a mild CENTER FORplace NATURAL SCIENCES force till it closes. Rotate lid gently in both directions to ensure an airtight seal; Ensure that the rim does not run out of grease but at same time do not use an excessive amount of grease. A thin uniform film is usually sufficient; Keep the lid upside down on removal but away from the workbench edge to prevent rollover; and Place a hot substance carefully inside after removal from the hot air oven. Keep the crucible with the lift ajar for a couple of minutes and then close the lid by sliding it to expel hot air so that the lid does not get blown out due to expansion of hot air and also prevent vacuum formation later which can make opening difficult. GUIDE QUESTIONS 1. List possible reasons for any discrepancy. Suggest ways to test your hypotheses. 2. Describe the determinate and indeterminate errors in an experiment. Prepared by: Olivar Reimos D. Barroga Instructor Submitted to: Regidor Almendral Instructor Submitted by: Allen Zyrix H. Espiritu Kevin Rye E. Perez Richelle Mateo Devalene P. Walat BSMLS 1C Copyright 2021. All rights reserved. No parts of this document may be reproduced in any form or by any electronic means, including information storage and retrieval systems, without permission in writing from the author, except by reviewers, who may quote brief passages in a review.