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110 Cards in this Set
- Front
- Back
Why is Food Analysis Important?
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Product development
New process evaluation Quality assurance Nutrition labeling Identifying problems with complaint sample |
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Food Analysis Applications
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Water Quality
USDA Nutrient Database Detect small particles |
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Steps in Analysis
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1. Select representative sample (Ch. 5)
2. Sample preparation (Ch. 5) 3. Perform the assay (entire text) 4. Calculate and interpret results |
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CHOOSING A METHOD
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Multiple methods available
Compare new method to a standard method Decision based on 1 Characteristics of the method 2 Objectives of the method 3 Composition of the sample |
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Objective of the measurement
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Nutrition labeling
Process control samples Moisture analysis – forced draft oven vs. moisture balance |
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Food matrix = sample chemical composition
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Food matrix affects the method performance
High fat or high sugar foods can interfere Digestion procedures and extraction steps often used Can a single method be used for multiple foods? |
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Method validity
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Method specificity, precision, accuracy, and sensitivity
Comparison with sensory data Nature of samples, if they are representative and number of samples analyzed Appropriate use of standardized equipment Use of “standard reference materials” or “check samples” |
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Examples of Official Methods
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AOAC International “Official Methods of Analysis”
American Association of Cereal Chemists (AACC) American Oil Chemists’ Society (AOCS) Standard Methods for the Examination of Dairy Products Standard Methods for the Examination of Water and Wastewater |
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Minerals:
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elements other than C,H,O, and N present in foods
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Nutritional value of food
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Enrichment, fortification increases content
Some processing methods decrease content Which minerals are required on a Nutrition Facts label? sodium, iron, calcium |
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Toxicity
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Lead, mercury, cadmium, aluminum, fluoride, selenium
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Food quality
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Affect cloudiness in beverages
Textural properties of fruits and vegetables Source of off-flavors (i.e. iron in milk) Hardness of water |
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Mineral analysis preparation
contamination |
ashing
Glassware Acid wash Water/reagents Use purest reagents available, including water Use a “reagent blank” |
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reagent blank”
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Contains reagents but not the sample to be analyzed
Used as baseline Result is subtracted from actual samples being analyzed |
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Factors that interfere with mineral analyses:
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pH, sample matrix, temperature, other analytical conditions, and reagents
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Stop interfering factors of mineral analysis
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Isolate the sample mineral
Remove interfering minerals Use a reagent blank Use a “background matrix solution” to make the standard curve Use a “spiked” standard curve |
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Methods of Mineral Analysis
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Titration
Colorimetric Methods Ion selective electrodes (ISE) Atomic absorption spectroscopy (AAS) Lab 4 Inductively coupled plasma-atomic emission spectroscopy (ICP-AES) Lab 4 |
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EDTA Complexometric Titration
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complexes are formed between EDTA and many mineral ions
pH dependent |
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Precipitation Titration
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titration reaction has at least one product that is an insoluble precipitate.
Ag+ + Cl- → AgCl (white precipitate) Mohr method Volhard method |
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Chloride Analyzer
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Titration
Relies on formation of AgCl Silver ions generated by passing a constant current between donor electrodes End point is detected by the use of sensing electrodes |
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Colorimetric methods
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Minerals react with another chemical (a chromogen) to form a colored product
Quantified by absorption of light at a specified wavelength using spectrophotometer Many methods exist |
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Ion selective electrodes
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Direct measure of cations
Not affected by sample volume, turbidity, color, and viscosity Simple (only requires electrodes and a pH meter) Limit of detection is usually 2-3 ppm Slow electrode response time at low concentration (below 10-4 M) Some electrodes have short operating life |
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Normality
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mequivalents/liter
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ppm
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part/wholeX1 million
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Titratable Acidity
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Equivalent to normality of the solution
Both ionized H+ and unionized H+; total potential H+. |
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Brix/acid ratio
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Titratable acidity
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pKa is
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the pH where [HA] = [A-]
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Henderson-Hasselbalch Equation
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pH=pKa+log (A-/HA-)
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Standard acid:
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Potassium acid phthalate (KHP)
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Standard base:
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NaOH
Needs to be standardized because NaOH is hygroscopic and can have impurities present. |
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% ACID
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(Ntitrant)(Vtitrant)(EqWt acid) X 100
--------------------------------------------------- (sample weight)(1000) |
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A buffer is a solution of
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a weak acid and its salt
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FDA
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Food and Drug Administration
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(FSIS)
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Food Safety Inspection Service
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(NIST)
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National Institute of Standards and Technology
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(NOAA)
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National Oceanic and Atmospheric Administration
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(NMFS)
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National Marine Fisheries Service
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(ATF)
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Bureau of Alcohol, Tobacco, Firearms, and Explosives
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government regulations for food published
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Code of Federal Regulations (CFR
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Why is a standard of identity useful?
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Prevents adulteration
Makes quality more consistent |
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FDA helps
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Inspects food processing facilities for compliance with GMP regulations and HACCP programs where required
Enforces nutrition labeling regulations Enforces standards of identity, quality and fill Works with other agencies regarding seafood safety (NMFS, EPA), imported products (CPB), interstate dairy industry (USDA Enforces regulations on pesticide tolerance set by EPA Responsible for food labeling |
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GMP regulations FDA
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Goal to prevent adulterated food
Include requirements for acceptable sanitary operation in food plants: |
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Standards of Identity
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Ingredients and levels contained in a food product
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Standards of Quality
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Minimum standards and specifications for some canned fruits and vegetables
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Standards of Fill
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How full a container must be to avoid consumer deception
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Hazard Analysis Critical Control Point
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HACCP
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HACCP
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Hazard Analysis Critical Control Point
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USDA mandatory inspection
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Meat and Poultry
Grains |
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EPA
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Establishes allowable limits for pesticide residues in food
Establishes standards for drinking water safety Establishes guidelines for effluent from food processing plants |
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International Standards and Policies
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Codex Alimentarius
ISO Standards JECFA Standards Food Chemicals Codex (FCC) |
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Spectroscopy:
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study of the interaction between electromagnetic radiation and matter
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light
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Particles of energy (photons) that move through space with wavelike properties
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Wavelike nature of light
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Explains light propagation
interference, diffraction and refraction |
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Particle nature of light
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Explains interaction of light with matter
Absorption and emission |
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Electronic
States of Matter |
Electron changing orbitals
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internal energy of a molecule
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depends on the electronic, vibrational, and rotational energies
Emolecule = Eelectronic + Evibrational + Erotational |
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internal energy of an atom
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depends on its electronic energy.
Eatom = Eelectronic |
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Accuracy
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How close a value is to the true or correct value
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Precision
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How reproducible, or how close replicate measurements become.
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Systematic error
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Results consistently deviate from the expected value in one direction or the other;
e.g., uncalibrated pipette, impure chemicals |
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Random error
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Results fluctuate in a random fashion; unavoidable
e.g., judging endpoint in a titration, using a pipette |
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Gross error (blunders)
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Results are scattered; easy to eliminate
e.g. missed adding reagent to one test tube |
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Sensitivity
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Indicates how little change can be made in the amount of unknown material before we notice a difference on a readout
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Detection limit
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The lowest possible increment that we can detect with some degree of confidence
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Curve fitting
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describe the relationship and evaluation between two variables
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Correlation coefficient (r)
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Defines how well the data fit to a straight line
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Sampling
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Obtaining a portion, or sample from a population
Should be representative of the population |
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Why Sample?
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Not usually feasible to test entire population
Makes analysis practical Estimates population (if done properly) |
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Sampling plan
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predetermined procedure for the selection, withdrawal, preservation, transportation, and preparation of the portions to be removed from a lot as samples
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Factors affecting the choice of a sampling plan
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Purpose of the inspection
Nature of the product Nature of the test method Nature of the population being investigated |
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Attribute sampling
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Certain characteristic is present or absent
e.g., C. botulinum |
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Variable sampling
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Quantitative amount on a continuous scale
e.g., percent fill of a container, or pH of a food sample |
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Single sampling plans
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Test one sample of specified size
Accept/reject decision |
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Double sampling plans
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Start with one sample
High or low quality = accept/reject decisions are made after one sample is evaluated Intermediate quality = a second sample is taken and both samples are used to make the decision |
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Multiple sampling plans
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Chart developed (see Fig 5-1)
Relates the cumulative number of defects to the number of samples taken from the lot Sampling continues until the number of defects crosses the acceptance or the rejection line |
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Risks Associated with Sampling
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Consumer risk
Vendor risk |
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Consumer risk
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Probability of accepting a poor quality population
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Vendor risk
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Probability of rejecting an acceptable product
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Probability Sampling
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Statistically Sound
Recommended |
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Nonprobability Sampling
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Use only with probability method is not feasible
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Problems in Sampling
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Sampling bias
Poor sample storage Mislabeling or nonpermanent marker Official or legal samples require sealing and chain of custody identified |
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Preparation of Samples
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Size reduction
Grinding – to reduce size and make homogenous Enzymatic inactivation Lipid oxidation protection Microbial growth and contamination |
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Why measure moisture
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Affects stability
Determines quality Concentration of food for shipping and packaging Ensures food meets Standard of Identity Necessary for nutritional value calculations Standardize results |
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to minimize moisture gains or losses
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Exposure of sample to open atmosphere
Heating (by friction) of sample during grinding Headspace in sample storage container Optimize speed of sample weighing |
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Forms of water
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Free (acts like water)
Adsorbed (held tightly to proteins) Water of hydration (Na2SO4 10 H2O) |
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Moisture analysis methods
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oven drying
distillation Chemical method-Karl Fischer Titration Physical methods |
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“Pan Handling”
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Store in desiccator
Only use tongs; fingerprints have weight |
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Sand pan technique (sand or diatomaceous earth)
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To control surface crust formation and disperse sample
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% total solids
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dry sample
-------------- X 100 wet sample |
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Distillation procedures
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Co-distilling the moisture in a food sample with a high boiling point solvent (usually toluene) that is immiscible in water
spices |
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Karl Fischer Titration
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Best method for many low moisture foods
Dried fruits and vegetables Candies, chocolate |
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Karl Fischer Titration
advantages disadvantages |
Rapid
Sensitive Does not use heat Incomplete water extraction (grinding size important) Atmospheric moisture can’t be present Moisture adheres to glass Interferences from certain food constituents |
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Physical methods
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Electrical methods
Refractometry Hydrometry Infrared Analysis Freezing Point |
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Electrical methods
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Dielectric constant is a measure of capacitance (resistance to an electric current)
% moisture is obtained from a standard curve Conductivity method Conductivity of an electric current increases with the % moisture in a sample |
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Hydrometry
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Science of measuring specific gravity or density
Pycnometer-most accurate |
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Refractometer
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Measures refractive index of a liquid
Based bending of light as it passes from one medium to another medium of different density |
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Infrared Analysis
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Measure of the absorption of near or mid-infrared radiation by molecules
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Freezing point
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Commonly used to determine if milk has had water added to it.
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Water activity
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Preferable to moisture content for
Predicting perishability Determining textural properties |
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Aw=
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partial pressure water above sample
--------------------------------------------------- vapor pressure of pure water at temp equilibrium rel humidity around sample/100 |
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Ash
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the inorganic residue remaining after either ignition or complete oxidation of organic matter in a foodstuff.
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Why measure ash
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Total mineral content of food
Part of proximate analysis for nutritional evaluation First step in specific elemental analysis |
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Ash content of food is usually
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<5%
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Dry Ashing
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Muffle furnace at 500-600 C
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Wet Ashing
(Oxidation) |
Combinations of nitric acid, sulfuric acid/hydrogen peroxide, and perchloric acid
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microwave muffle furnaces
Advantage disadvantage |
Decreased time for ashing (minutes instead of hours
Limited number of samples can be ashed at one time Expense of equipment? |
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Dry Ashing
Advantages Disadvantages |
Safer than wet ashing
No attention needed once begun Large numbers can be done at once No added reagents or blank subtraction Time (12-18 hr or overnight) Expensive equipment (relative to wet ashing) Loss of volatile elements and interaction with crucible (list of minerals lost on p. 106) |
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Wet Ashing
Advantages Disadvantages |
Minerals usually stay in solution
Little loss from volatilization because of lower temperature Short time Requires constant operator attention Corrosive reagents Only small numbers of samples done at one time Special hood required for perchloric acid, since it’s explosive |
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Name the oranization that sells standard reference or check samples for cereal products
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American Association of Cereal Chemists
(AACC) |
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Which US government agency provides grading services for a variety of foods?
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US Department of Agriculture (USDA)
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