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QUALITY CONTROL LAB III.

GRAVIMETRIC
- Based on wt solution, weight of a substance of
ANALYTICAL known identity
• Qualitative - Prepared by extraction, precipitation or other
- what is present? needs of constituents to be determined either
- Reveals the chemical identity of the species in in natural state or in the form of definite
the sample compound of known composition and weighing
- Compounds present, composition the resulting product
• Quantitative
- Quantify IV. SPECIAL METHOD
- Establishes the relative amount of one or more - Distinct type of technique
species in the sample - Assay of alkaloids or other classes of secondary
- How much is present? metabolites

Methods of Quantitative Analysis Laboratory Operations and Techniques:


I. VOLUMETRIC ANALYSIS
- Determination of the volume of a solution with Analytical Balance
known conc. Required to react with a given • Spirit Bubble
amount of substance to be analyzed - to check if at the center
- to calibrate
i. 5 types of volumetric analysis • Accuracy
a. Neutralization - Indicates closeness of the measurement to its
o Reaction of acid and base true or accepted value
o Product: Salt • Precision
o By-product: Water - For the reproducibility of the measurement
• Capacity
b. Precipitation/Precipitimetry - Maximum weight that a balance can measure
o Forming precipitate (insoluble • Sensitivity
compounds in solution - Minimum weight that will produce a
measurable response
c. Complexometric Reaction • Readability
o Forming insoluble complexes with Ca or - Smallest discernible scale division
other polyvalent ions - Rough balance (0.1)
- Cent-o-gram (0.01)
d. Redox Reactions
o Count the # of e- gained or loss Macro - larger capacity (more than 0.1g)
Semi micro - sample is 10-100mg
e. Specific Reactions
o Permanganate Manual & Digital
o Ceric sulfate • Mettler Balance
o Iodometry/Iodimetry • Ohaus
• Sartorius
II. PHYISCOCHEMICAL
- based on specific (physical/chemical) property Types of Weighing:
a. polarimetry • Direct Weighing
b. refractometry o Total weight
c. thermal conductivity o Weight of volumetric flask
d. electrometry • Weighing by difference
e. spectrophotometry o Using hydroscopic or volatile substance
f. chromatograph o Initial wt – final wt

C. ANDAL | 3IPH
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Volumetric glasswares – increase degree of accuracy • w/o frosted bond
2 types: - no need to blow (calibrated)
• TD (To deliver)
- Serological pipette Specific types of pipette:
- Buret a. Volumetric or Transfer pipette
- To deliver specific or calibrated volume - Has one calibration
b. Ostwald Falling Pipette
• TC (to contain) - Similar to volumetric but the last drop needs to
- Designated to contained a specific volume be blown out
c. Measuring/Mohr Pipette
Burets – long tube with calibrating - Deliver various volumes
• Mohr d. Serological Pipette
- Can contain bases - Deliver various volumes but the last drop has to
- Base buret be blown out
- Rubber pinch cock e. Syringe Pipette
o NaOH - Can deliver fix or various volume in a range of 1-
o H2C2O4 1000ml
o KSCN - Dispensable pipette tips
o Na2S2CO3
• Geisssler acid buret Volumetric flask
- Glass stop cock - 1 calibration
- Red tip - parts: neck and bulb
o HCl
o AgNO3 Steps on how to clean:
o KMnO4 1. rinse with tap water
o I2 2. Wash with liquid detergent + water
• Teflon valve 3. Rinse with tap water
- Used for both acid and base 4. Distilled H2O
- Universal 5. Small amount of solution
*return to reagent bottle
Techniques (Buret) *excess after titration – return
1. Shake the reagent bottle (do not use
intermediate container) Titration techniques
2. Close buret 1. Excess
3. Excess 2. Fill tip
4. Release to fill the tip 3. Zero 0.0ml
5. Transparent – lower meniscus 4. Read – instructor
6. Colored – upper meniscus *with the aid of marker
7. Touch the inside – to remove drop 5. Erlenmeyer with analyte and indicator (gives
color change because of TH)
*wicking out – do not use tissue, prevent parallax error 6. Shake Erlenmeyer to prevent settlement
7. Let go hanging drop
Pipette 8. Wash bottle – spray the sides
- Accurately transfer specific weight of liquid
Phenolphthalein
2 types: (General) Initial – pink Acidic – colorless
• w/ frosted bond Neutral – light pink Basic – dark pink
- the last drop is needed to be blown out (use
aspirator)

C. ANDAL | 3IPH
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