Helps in separating immiscible liquids like oil and water into two samples
Separatory funnel
Mixtures of liquids and solids are usually separated prior analysis by
filtering
decanting
centrifuging
Pre-treatment of solid samples prior analysis
Leaching and extraction of soluble components
Filtering of mixtures of solids, liquids and gases to leave particulate (solid) matter
Grinding
Decomposition and dissolution of solids during sample preparation
Acid treatment using oxidation
Fusion technique
Dissolution using ultrasound&appropriate solvent
Simple dissolution
Reliability of the results
Decreases with a decrease in the level or concentration of the analyte
Properties of nitric acid making it the preferred acid for digesting samples for the analysis of metals
Acts as a strong acid
Acts as an oxidizing agent
Does not form insoluble compounds with metals/nonmetals
Primary sample preparation method for organics
Sonication
Acid-digestion
Extraction
Possible sources of contamination during sample preparation
Reagents (tracers)
Glassware/equipment
Cross-contamination between high- and low-activity samples
Containers that should not be used for dry ashing
Glass and plastic
The size of the sample taken for analysis depends on
the concentration of the analyte
equipment to be used
specific tests
Equipment commonly used to homogenize the contents of an open beaker
Magnetic stirrer
V-blenders
Ball and rod mills
tube rotator
The maximum holding time for acid preserved samples that will be subjected to determination of metals
3 months
Laboratory sample
A fraction of the sample actually used in the final laboratory analysis
Matrix effect
A change in the analytical signal caused by anything in the sample other than analyte
Matrix
Medium containing analyte
The total error of an analytical result is the sum of
sampling
sample preparation
analytical errors
The holding time for samples for metal determination preserved using nitric acid, 4 mL of dilute 3:1
28 days
When samples cannot be dried because they decompose at the temperatures necessary to drive off the water, the samples can be analyzed as
wet basis
dry basis
received basis
Soxhlet extraction
Organic components in solid samples are extracted from the matrix by continuously washing the solid with a volatile solvent in a specialized piece of glassware
Nonaqueous
In liquid-liquid extraction, if a drop of water dissolves in the top layer, the top layer is nonaqueous
Sampling
Process by which a sample population is reduced in size to an amount of homogeneous material that can be conveniently handled in the lab in which the composition is representative of the population
Error in sampling and the sample preparation portion of an analytical procedure
Considerably higher than that in the methodology
Homogenization during sample preparation can be achieved using
mechanical devices (mixers, blenders, etc.)
enzymatic methods
chemical methods
Glass container is not suitable for
inorganic trace analyses
oil and grease determination
microbiological analyses
To increase/decrease analyte concentration, pre-concentration is needed for almost all trace analysis, _______ is used for the analysis of highly contaminated samples so the concentration falls within the calibration range
dilution
Chemical derivatization
Used to increase or decrease volatility for GC and HPLC analysis
Acid digestion via hot-plate digestion or microwave-assisted is one way of sample preparation in the analysis of
Total metal
Bioactive compounds
Alcohols
Sugars
Nitric Acid
Used in GFAA (Graphite Furnace Atomic Absorption) as it does not interfere with Cl-
Partitioning of analytes between water phase and organic phase
Liquid-liquid extraction
Soli phase extraction
Ultrasonic extraction
Pressured Fluid Extraction (PFE)
The amounts of all constituents in the samples were determined
Complete (or ultimate) analysis
Partial analysis
Elemental analysis
Macro analysis
Implies that the constituent determined was present in high concentration
Gravimetric analysis
Quantitative chemicall analysis of weighing a sample, usually of a separated and dried precipitate
ACS grade
A chemical grade of highest purity and meets or exceeds purity standards set by American Chemical Society
Reversible reactions
Bidirectional harpoons or double arrows (⇆) should be used to indicate
A few ways in which solution composition can be described are as follows
Molarity
Normality
Molality
Solvent
The substance which does the dissolving and must be
In the preparation of 1 liter of 1.0 N acid from 35% Hydrochloric Acid, what weight of the impure acid should be taken, assuming standardization in the recommended manner?
g=(1 eq.wt. HCl/li x 1 liter x 1mole/1 eq. wt. HCl x 36.45 g HCl/mole)
a. 101.29
b. 113.29
c. 111.29
d. 124.89
A few ways in which solution composition can be described are as follows
Molarity
Normality
Molality
All of the above
Solvent
The substance which does the dissolving and must be greater than 50% of the solution
Used to measure volumes approximately, typically with errors of several percent except for one