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FST 202 FOOD ANALYSIS

1. Proper use of desiccators and desiccants a. To open the desiccator, slide the lid gently, i.e. horizontally, and hold it on level while transferring samples in and out of it with a tong or pincher. Close in similar manner. b. If glass to glass scraping is detected, rub a small amount of silicon grease all around the flat surface of the lid and slide back and forth to ensure distribution. c. Close the desiccator immediately after each use. It must not to be left open except to transfer samples in or out of it. d. The desiccator contains a plate with holes over a screen which covers granulated anhydrous calcium sulfate, a desiccating or dehydrating agent. It should be bluish at all times, replace when about 20% has turned pinkish or reddish. e. Dry the spent desiccant in 105C until color returns to blue. Store in dry, airtight container ready for use. 2. Proper way of filtering liquid or suspension using filter paper a. Use lint-free, ashless filter paper for analytical determination, of appropriate grade depending on nature of liquid, or of precipitate/sediment to be filtered out. Use lint-free paper for general use. b. Fold filter paper using gloved hand to avoid contamination using any of as follows: b.1. the quarter fold: i. Fold the round piece of filter paper in half and crease it. ii. Fold again and crease to produce a quarter circle. iii. Separate one outer layer of paper from the other three (not two and two) and widen the the opening by squeezing slightly together at the creases. iv. Place the conical shaped piece of filter paper into a glass or plastic funnel and wet slightly with distilled water from a wash bottle. b.2. the 8 or 16-segment paper: For a more efficient flow, the paper has to have more exposed area with the liquid and less contact area with the funnel. v. Follow steps i & ii in b.1. Fold each quarter outward in two and crease with the adjacent fold. This makes an 8-fold paper. vi. To make a 16-fold(most flow-efficient), fold each 8-segment into two and crease with the adjacent fold. It should appear like a conical zigzag pattern. c. Insert the holder into a filtering rubber or cork into the filtration flask. Allow untight fit of the stopper to facilitate flow. If using filtration stand, insert the funnel into the slot and orient the tip such that it is adjacent the wall of the filtration vessel.

d. Transfer liquid using a glass rod up to a maximum level of at least 3 mm from the paper edge. e. Loosely cover the funnel with watch glass and the filtration vessel with a clean, lint-free cover with hole. 3. Directions and guidelines for using pipet a. Care and storage: i. Examine each pipet for chipping. Minor chip around the tip is usually fine to use, however, once the fracture has affected majority of the wall such that liquid path is compromised, it is no longer fit for use. ii. Washing the pipets: a) Rinse off the adhering liquid thoroughly under running water. b) Completely soak in detergent solution taking care of the tips. If using pipet cylinder, soak them tip side up. Use warm water or alcohol to dissolve oily or fatty films before using detergent. c) Rinse thoroughly under running water and finally rinse with distilled water. d) When solid dirt accumulates in the tip, remove it immediately by poking with a thin, non-scratching wire usually supplied with the pipets or burettes. Wash the material out through the nozzle using a rubber bulb or fill the fipet with water and reverse-drain through the neck to wash the particle out the other end. Do not let the material dry to avoid adhering permanently on the pipet wall. b. Handling & use: i. In drawing liquid, squeeze the suction bulb before pressing its hole against the pipet mouth. This step creates an air-tight seal between bulb and pipet mouth. ii. Place the tip of the pipet in the solution to be drawn up and slowly release the bulb. Draw the liquid until the meniscus is way above the calibration mark or the graduation. Remove the bulb and quickly cover the pipet mouth immediately with your free index finger. iii. Exercise care not to allow the tip of the pipet to break the surface of the liquid while drawing in the solution since this will result to sudden decrease in viscosity at the pipet tip which will cause a large amount of liquid to enter and contaminate the inside of rubber bulb resulting from the entry of air pushing the liquid up beyond the mouth of the pipet. iv. Make sure that line of sight is perpendicular to the length of the pipet. Allow a tiny amount of air by slightly releasing the finger until the meniscus drops to the calibration mark or desired level. v. Remove the pipet from the reagent solution, wipe wetted external portion with clean absorbent paper and transfer the liquid to the receiving flask, allowing the liquid to run against the wall. Let the liquid drain by itself. vi. Unless marked with the word BLOWOUT and/or a white enamelled (etched or sandblasted) band, 3 to 5 mm wide approximately 15-20mm from the top of the suction tube, a pipet should

not be "blown out" to eject all liquid at the tip because they are calibrated in a manner that takes into account the solution which remains at the tip due to surface tension.

4. Directions and guidelines for using buret a. Maintenance and storage: i. Wash off the remaining solution in the buret by repeated filling and draining of water while petcock is removed. Soak the insides with detergent solution by re-inserting the petcock. If poor drainage is encountered such that it shows droplets after drying, use buret brush or dichromate/sulfuric acid cleaning solution and wash normally. As in the pipet, remove any stubborn solid dirt by inserting thin wire through the nozzle and flushing out through any of the openings. Store away tip side up in the buret cabinet, placing one ear of the petcock valve in designated hole to prevent from falling out when cabinet is opened. In the absence of buret cabinet, mount buret clamp on iron stand to hold the buret tip side up.

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b. Handling and use: i. Rinse at least twice with the solution with which the buret is to be filled. If wet, rinse with water and then a minimum of 3 times with the solution to be used. About 1/5 of the volume of the pipette or burette is adequate for each rinsing. Fill the buret through the top of the column and drain until desired volume is attained as reflected by the lower meniscus for clear liquids or the upper meniscus for dark liquids. Before using the buret, ensure absence of bubbles in all parts usually encountered in the nozzle portion. Completely fill the buret, fully open the valve, and let the liquid to drain until the bubble is removed. Other way is to suck the air with a rubber bulb while draining until the liquid is clear of bubbles. Dispense liquid gradually unless the expected volume is pre-validated, taking care not to overshoot the end-point. When reading a buret the line of sight must be in a direction perpendicular to the buret column. Negate the variability of the background by using a buret card a white card streaked with at least 1-inch wide black ink, facilitating a higher precision read-out by the constant dark reflection against a white background. Ensure that the column is filled with the solution up to full graduation before a series of titrations. Always begin titration by reading original volume and end by reading the final volume.

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5. Directions and guidelines for using volumetric glasswares Volumetric glasswares are precision glasswares capable of measurements of volume that are good to four significant digits and are consequently expensive. They are characterized by long slender necks with a single graduation mark on them. Any glassware with several graduation marks is not volumetric. a. Maintenance and storage: i. ii. Do not expose any volumetric glassware to sources of heat since such exposure will adversely affect the calibration, do not dry any volumetric glassware in a drying oven. Clean the glassware before using. It must drain in such a manner that a smooth film of solution adheres to the inside, there must be no beading or droplet formation on the inside walls of the vessel. Ensure beading is eliminated by using either of: a) A mixture of equal parts of a saturated solution of potassium dichromate and conc. sulfuric acid. b) A mixture of equal parts of 30g/l solution of potassium permanganate (KmnO4) and a 1mol/l solution of sodium hydroxide (NaOH). Removed the resulting residue of MnO2 with dilute HCl or oxalic acid. Rinse with distilled water and ascertain if the walls are sufficiently clean otherwise, repeat the procedure. b. Handling and use: i. Before use, rinse at least twice with small portions of the solution to be measured. When filling, the rising liquid meniscus shall not change shape i.e. it shall not crinkle at its edges. After over-filling and drawing a little liquid, the meniscus shall be smoothly concave and not crinkle at the edges. When using a volumetric flask, dilute the solution stepwise. a) Add the solution to be diluted into the flask, and add the diluent (usually distilled water) to fill the flask about two-thirds. Ensure that any reagent on the ground glass lip is rinsed down. Swirl the flask to obtain utmost mixing or dissolution. Add the diluent so that the bottom of the meniscus is even with the middle of the calibration mark at eye level. b) If there are any droplets of water on the neck of the flask above the meniscus, blot these out with a tissue paper. Dry the ground-glass stopper joint. c) The solution is then thoroughly mixed. Keeping the stopper on securely by using the thumb or palm of the hand, invert the flask and swirl or shake it vigorously for 5 or 10 seconds. Turn right-side up and allow the solution to drain from the neck of the flask. Repeat 10 times. iii. iv. Do not shake or blow out volumetric pipets since its design allow retention of the tip volume. In delivering hold the pipette vertically with the tip touching the side of the vessel to allow smooth delivery without splashing and so that the proper volume will be left in the tip.

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6. Procedures on determining proximate composition of food Determining proximate composition of food is analysis of foods and feedstuff for protein, fat, mineral salts, and soluble carbohydrate calculated by subtracting these values from the total. To carry out the analysis: a. Set the protocol. b. Sample the food. c. Prepare the sample in readiness for extraction of the chosen analyte or compound of interest (COI). Includes such processes as grinding, digestion, and centrifugation. The stage includes standardisation. d. Extract the COI, making available a less complex, and usually more concentrated compound or substance of interest via physical, chemical, or biochemical methods. e. Separate from, or remove substances interfering with the detection of the COI in the extract. The step is conducted by chromatographic and electrophoretic processes where the main objective is not to remove or extract something for further stages of analysis, but to finally resolve components of mixtures for detection and identification. f. Detection (recognition or visualisation), and identification and/or quantification of the COI. The process is characterized by signal recorded when a component of the sample is registered (recognised, standardised or calibrated) above a base line, and the signal content is converted into qualitative or quantitative information.

7. Proper use of pH pen A pH pen is actually a portable pH electrode, encased in chemical resistant plastic, usually powered with battery, and equipped with a digital display. It does not have a temperature compensator and is used commonly for field analytical work. a. As in table-type pH meter, the electrode must first be calibrated before daily use, with Buffer 7, then Buffer 4 if sample is acidic or Buffer 10 if sample is basic. b. After calibration, rinse the electrode with distilled water. Pat dry the excess liquid with clean tissue paper. c. Rinse with the sample to be analyzed by immersion in small amount of sample and discard. d. Proceed with analysis of the sample by swirling gently until electrode output has stabilized. e. After each use, rinse with distilled water. Pat dry the excess liquid with tissue paper and let airdry before storing in its hard plastic jacket.

References: Shugar, Ballinger, and Dawkins, Chemical Technicians Ready Reference Handbook, p. 565-571 2010, Maryland Science Safety Manual, Chemicals: Managing, Handling, and Disposing 2010, Royal Society of Chemistry, London 2010, Ulrich de la Camp & Oliver Seeley, Helpful Hints in Use of Laboratory Equipment 2003, Reagecon Diagnostics Ltd. GFS Chemicals, www.gfschemicals.com/