CHEM 212

CHEM 212
Quantitative Analysis
Learning Outcomes
 Learning Outcomes
Module 1 - Critical Thinking and Problem Solving
Lecture 1 - Introduction
- Understand the core principles of the course regarding admin, EQHR, structure, methods, etc.
- Know where to go to find more information

Lecture 2 - Critical Thinking

- Discuss what analytical chemistry is
- Summarize the definitions given and explain what it is in your own words
- Summarize the key principles of the scientific method
- Discuss why the scientific method allows us to answer questions and provide context to
data
- Define “critical thinking” for this course
- Understand the basic concepts of data collection for surveys
- Discuss sources of error or subjectivity associated with methods of data collection for
surveys
- Discuss the pros and cons of methods of data collection for survey

Lecture 3 - Sampling
- Explain how samples are prepared for lab analysis
- Terminology:
- Sampling
- Lot
- Bulk sample
- Laboratory sample
- Aliquots
- Look at sample preparation diagram
- Compare and contrast the different types of sampling plans
- Different types of sampling methods:
- Random
- Judgemental
- Systematic
- Systematic-Judgemental
- Judgemental-Random (Stratified)
 - Convenience
- Explain why a certain sampling plan has been chosen for gathering a particular type of
sample
- Know the types of sampling p
- Also relate to storage of samples

Lecture 4 - Measurements and Errors

- Define:
- Accuracy
- Precision
- Repeatability
- Reproducibility
- Error
- Uncertainty
- Systematic Error
- Random Error
- Gross Error
- Absolute Uncertainty
- Relative Uncertainty
- Percentage Relative Uncertainty
- Use the above definitions to interpret and classify different types of data and uncertainties
- List different methods for proving the accuracy of an analytical method or measurement
- Calculate:
- Relative uncertainty and percentage relative uncertainty
- Random errors using uncertainty propagation

Lecture 5 - Significant Figures

- Describe the meaning of a number relative to its number of significant figures
- Use the rules for rounding numbers to accurately round numbers to the required number of
significant figures
- Perform the following calculations:
- Addition/subtraction using the correct number of sig figs
- Multiplication/division using the correct number of sig figs
- Logs/antilogs using the correct number of sig figs
- Calculations using the correct number of sig figs and taking uncertainty of
measurements into account (The Real Rule)

Lecture 6 - Statistics and Data Analysis

- Define:
 - Mean
- Standard Deviation
- Normal Distribution (and why it’s used to model the underlying spread of data)
- Correlation and Variable (in the context of science)
- Also explain why correlation does not equal causation (p-hacking, data
dredging)
- Raw Data and Processed Data (explain the difference between them)
- Calculate:
- Propagation of uncertainty calculations from systematic uncertainties
- Explain how error bars allow us to plot the mean of a set of measurements together with a
value for the uncertainty of the measurement
- Describe how the way data are plotted can be misleading
- Understand that all statistical methods have limitations and may be misleading
- Describe possible sources of cognitive bias in data analysis and mitigation strategies
- Describe the concept of “statistical significance” and how it can be shown using statistical
methods

Module 2 - Liquids and Their Use in Analytical

Chemistry
Lecture 7 - Acids and Bases
- Calculate:
- Equilibrium constants
- pKa of an acid from the pH
- pH, kA and pKa
- Apply Le Chatelier’s principle to predict equilibrium behaviour
- Define Bronsted-Lowry acids and bases
- Describe strength in terms of acids and bases

Lecture 8 - Buffers and Solutions

- Explain what a buffer is
- Calculate the pH of a buffer solution of known concentration
- Define the Hender-Hasselbach equation
- Use the Hunderson-Hasselbach equation to calculate pH
- Define:
- Solution
- Molarity
- Weight percent and volume percent (including v/v, w/v and w/w nomenclature
- Calculate:
 - Use the above definitions to perform calculations
- Calculate solution dilutions in one or more steps (using the dilution formula)
- Apply knowledge about uncertainties to experimental situation involving solutions

Lecture 9 - Separation Techniques

- Define:
- Matrix
- Analyte
- Interferent
- Sample preparation (explain)
- Different types of separation (based on size, mass, density, change of state,
partitioning between phases)
- Give examples and real life uses of each separation technique

Lecture 10 - Liquid-Liquid Extraction

- Define:
- Liquid-liquid extraction
- Distribution coefficient
- Describe how it’s used in pharma and other real life examples
- Calculate:
- KD and q
- Describe the effect that pH has on KD and q
- Perform calculations on D and q for acids and bases

Module 3 - Quality Assessment and Calibration

Methods
Lecture 11 - Quality Assurance and Calibration Methods
- Define:
- Quality assurance and the quality assurance process.
- Describe the importance of quality assurance in analytical chemistry.
- Different types of standards used for calibration curves.
- Sensitivity
- Specificity
- Limit of detection, False Positive, False Negative
- Describe the relationship between the detection limit, false positives and
false negatives
 - Numerically describe the significance of false positive and false negative
results.
- Limit of quantitation
- Method blank
- Reagent blank
- Field blank
-
- Calculate:
- Perform calculations using the detection and quantitation limits.
- Perform calculations involving calibration curves

Lecture 12 - Standard Addition

- Describe what standard addition is and why it is used
- Describe the matrix effect
- Describe the methods of standard addition for variable and constant total volume
- Calculate:
- Variable total volume standard addition experiments
- Constant total volume standard addition experiments

Lecture 13 - Internal Standards

- Define:
- Internal standard and why it is used
- Calibration curve
- Describe how to build one using internal standards
- Compare and contrast the different methods
- Calculate:
- Calculate for experiments using internal standards

Module 4 - Analytical Chemistry Instruments

Lecture 14 - Chromatography
- Define:
- Chromatography
- Basic states for separation of two solutes
- Different types of chromatography and examples
- Analyse a chromatograph in terms of retention time, separation factor and
retention factor
 - Describe the relationship between the retention time and partition
coefficient
- Describe the resolution of chromatographic peaks
- Physical basis of chromatography
- Retention volume
- Calculate:
- Retention time
- Separation factor
- Retention factor
- Retention volume
- Resolution of chromatographic peaks

Lecture 15 - Introduction to HPLC and GC

- Describe how HPLC works:
- Describe mobile and stationary phases
- Describe how samples are injected into an HPLC
- List the typical detectors used in HPLC experiments
- Describe how a gas chromatograph works
- Describe how GC is used for qualitative and quantitative sample analysis
- Describe accuracy, precision, sensitivity and selectivity of GC

Lecture 16 - Introduction to Mass Spectrometry

- Describe how a mass spectrometer works
- Describe electron and chemical ionisation methods for MS
- Define:
- Nominal mass
- Monoisotropic
- Molecular ion
- M+1
- Use it to predict the number of carbon atoms in the analyte
- Base peaks
- Nitrogen Rule
- Describe how a GC-MS or an LC-MS work

Lecture 17 - Introduction to Microfluidics

- Define:
- Microfluidics
- Describe advantages associated with microfluidic devices
- Describe how microfluidics devices are fabricated
 - Describe what a microfluidic droplet is and why they are used
- Briefly describe some microfluidic devices for analytical chemistry
- Laminar flow
- Turbulent flow
- Reynolds number
Practice Problems
 Practice Problems
Module 1 - Critical Thinking and Problem Solving
Lecture 1 - Introduction
- Understand the core principles of the course regarding admin, EQHR, structure, methods, etc.
- Know where to go to find more information

Lecture 2 - Critical Thinking

Lecture 3 - Sampling
- For the following questions, which sampling method is being used, why, and what are the
sources of error/subjectivity associated with the choice of sampling strategy:
1. A student researcher samples soil only from shaded areas of the field, believing
those are most likely to retain moisture and show different nutrient levels.
2. Every 50th bottle of cough syrup is pulled from the production line and tested for
sugar concentration
3. Analytical chemists group drinking water into urban supply, rural wells, and bottle
sources, then randomly sample within each group for pH testing.
4. A quality control inspector selects glass beakers with visible scratches for further
stress testing in a production plant
5. In a chemical warehouse, inspectors decide that the oldest drums of ethanol are
most likely to degrade and test those, repeating this monthly.
6. A technician tests the first 5 mL of gas coming from a pipeline at fixed 10-min
intervals over 24 hours.
7. In a chromatography lab, an analytical chemist tests the vials sitting at the end of
the bench because they’re closest to reach.
8. Researchers number all reagent bottles in stock and use a lottery method to select
15 for purity analysis.

Lecture 4 - Measurements and Errors

1. What is the percent relative uncertainty of a burette reading of 24.35 +/- 0.02 mL?
2. The uncertainty of a pipet is +/- 0.05 mL. What is the range of the true value of a reading of
17.23 mL
3. The volume delivered by a burette is the difference between final and initial readings. If the
uncertainty in each reading is +/- 0.02 mL, what is the uncertainty in the volume delivered?
Lecture 5 - Significant Figures
1.

2.

3.

4.
5.

6.
7.

8.
Lecture 6 - Statistics and Data Analysis

Module 2 - Liquids and Their Use in Analytical

Chemistry
Lecture 7 - Acids and Bases

Lecture 8 - Buffers and Solutions

Lecture 9 - Separation Techniques

Lecture 10 - Liquid-Liquid Extraction

Module 3 - Quality Assessment and Calibration

Methods
Lecture 11 - Quality Assurance and Calibration Methods
- Define quality assurance and the quality assurance process.
- Describe the importance of quality assurance in analytical chemistry.
- Numerically describe the significance of false positive and false negative results.
- Define sensitivity, specificity, limit of detection, limit of quantitation, method blank,
- reagent blank and field blank.
- Describe the relationship between the detection limit, false positives and false
- negatives.
- Perform calculations using the detection and quantitation limits.
- Define the different types of standards used for calibration curves.
- Perform calculations involving calibration curves
Lecture 12 - Standard Addition

Lecture 13 - Internal Standards

Lecture 14 - Chromatography

Module 4 - Analytical Chemistry Instruments

Lecture 14 - Chromatography

Lecture 15 - Introduction to HPLC and GC

Lecture 16 - Introduction to Mass Spectrometry

Lecture 17 - Introduction to Microfluidics

Module 1
Tab 8
Lecture 3 - Sampling
 Lecture 3 - Sampling
Stuff Learned from Chocolate Conundrum
- The scientific asked matters
- Sometimes the right question isn’t asked or is vague
- Scientific method encourages refinement of question dependent of data
- There are usually several (analytical) chemistry techniques that can answer the same question
- There is no one correct answer, method, or analytical technique
- Methodology for data collection affects the usefulness of the data in answering the initial
question

Scientific Method Related to Chocolate Conundrum

1. Identify and define problem
a. e.g. what is the most popular type of chocolate in Switzerland?
i. Most sold? Type of chocolate? People currently in country orrr??
2. Define experimental procedure
a. List possible data collection techniques to be used
b. Determine the pros and cons of each method in relation to your constriatns
c. Pick one or more pros and cons, then define exact method to be used for data
collection
3. Conduct experiment and gather data
4. Analyze experimental data
5. Propose solution to problem

Communicating Research
Facts Don’t Change Minds
- Social/hive mind behaviour (open space for debate and dialogue), values, emotions and
experience change people’s mind
- Social connectivity has a big impact on changing one’s mind
- Still keep facts, but don’t persuade using just facts

Sampling
- Sample data has to be representative of the whole population
 - Population: the entire data set that fits your parameters
- Sample: A subsection of the population selected using a pre-defined method that
can be used for analysis

Homogenous and Heterogenous Samples

- Sampling strategies depend on the composition of the material
- Homogenous: same composition everywhere in the material
- Heterogenous: different composition from place to place in a material
- Random: areas of different composition completely random
- Will likely always include the “different” data
- Segregated: Chosen percents of different data
- May not include a “different” type of data

Collecting a Lab Sample

Sampling and Sample Preparation
1. Sampling
2. Prepare sample
3. Separate sample into aliquots to do multiple tests
Terminology
- Sampling: the process of collecting a representative sample of analysis
- Lot:
- Bulk Sample:
- Laboratory Sample:
- Aliquots:

Storage of Samples
- Think about how you’re storing the samples, not just where you’re storing it

Types of Sampling Plans

- Want to have an unbiased estimate of the target population’s properties
- Types of Sampling Methodologies:
- Random: Fully unbiased, most objective sampling method
- True randomness is hard to achieve
- e.g. Placing 20 students names into a hat for a survey and drawing a name
randomly
- Judgemental: Using prior information about target population to help guide sample
selection
- More biased than random sampling, but less sampling involved
- e.g. Testing PCB levels in fish based of a certain tissue level, so if not reaching
that level, won’t bother testing it
- Systematic: Sampling the target population at regular intervals in space (location) or
time
- If the population has a periodic trend, this type of sampling will lead to
significant bias is sampling frequency too small
- e.g. In a hospital, having to test blood samples, so need to test over time.
Need to make sure that spacing captures the data we want
- Systematic-Judgemental: Prior knowledge about system guides systematic sampling
plan (guides the interval that samples are taken)
- Judgemental-Random (Stratified): Used for target populations consisting of distinct
units or strata to minimize sampling bias
- e.g. taking air quality samples in LA, so take sample at ground level, at building
level, then well above the city as a control group
- Convenience: Sample sites selected using criteria other than minimizing sampling
error and variance
- Predetermine sites
Lecture 4 - Measurements and Error
 Lecture 4 - Measurements and Error
Accuracy and Precision
- Accuracy: Describes how close a measured value is to the “true” value
- Precision: Describes the reproducibility of a result

Demonstrating Accuracy
- Ways to demonstrate accuracy:
- Measure with reference to a control sample
- Compare results from two or more analytical methods
- Should agree within expected precision
- Analyze a “certified reference material” in matrix similar to unknown
- Value of reference material should be within precision of
method
- Matrix = have sample in something (the containment
material)
- Analyze blank sample spiked with known addition of analyte
- e.g. standard additions
- Example: Is my blood glucose reading correct?
- Manufacturers include “control” samples for users to help test
- (Aim for an accurate result based of measurement of blood
glucose levels)
- Readings may indicate serious health issues, poor technique, or malfunctioning meter

Certified Reference Materials

- Standard Reference Materials: Certified materials with set value used to assess accuracy of
an analytical procedure
- Certified with painstaking care at National Standard laboratories
- e.g. anticonvulsant drugs for patients with epilepsy require specific concentration in blood
serum
- FILL IN

Additional Definitions
- Repeatability: Describes the spread in results when one person uses one procedure to analyze
the same sample by the same method multiple times
- Similar to precision kinda, but used in different contexts
 - Reproducibility: Describes the spread in results when different people in different labs use
different instruments each try to follow the same procedure

Uncertainty and Errors

- Error: The difference between the true and the measured values
- It is a measure of accuracy
- Three Types:
- Systematic (Determinate) Error: FILL IN
- e.g. Something wrong with instrument, getting same value or
something
- Can be highly precise but not accurate
- Random (Indeterminante) Error: FILL IN
- Spread in measurements
- Gross (Blunder) Error: FILL IN

Defining Experimental Errors

- Absolute Uncertainty: Expresses the margin of
uncertainty associated with a measurement
- Examples:
- Gilson Pipetman: P1000L
- Ruler: +/- 1mm
- Is not a systematic error, but a range
- Systematic Error: Consistent bias in measurements associated with a flaw in
instrument that always shifts in the same direction
- Maximum Permissible Errors
- Relative Uncertainty: Compares absolute uncertainty with the size of
measurement
Worked Examples
Uncertainty Propagation from Random Error
- For addition and subtraction: use absolute uncertainty
- For multiplication and division: use relative uncertainty
Lecture 5 - Significant Figures
 Lecture 5 - Significant Figures
The Importance of Significant Figures
- Significant Figures: The minimum number of digits needed to write a given value in scientific
notation without loss of precision
- Also the “digits that carry meaning contributing to its measurement resolution”

Rules about Zeroes

- Zeroes are significant when they occur:
- In the middle of a number
- At the end of a number on the right side of the decimal point

Significant Figures in Calculations

Rounding Off
- Only round in your final answer to avoid rounding errors
- In the case where the number is exactly halfway, round to the nearest even digit
-

Addition and Subtraction

- If the numbers being added or subtracted have an equal number of digits, the answer goes to
the same decimal space as in any of the individual numbers
- Round to the lowest number of decimal places of the individual numbers
- For addition/subtraction in scientific notation, all numbers should be expressed with the
same exponent, then figure out the rule to use
Multiplication and Division
- Round up/down by the lowest number of sig figs in the question\
- Doesn’t include scientific constants

Logarithms and Antilogarithms

- Characteristic: Digits to the left of decimal point
- Mantissa: Digits to the right of decimal point
- Sig Fig Rule: The number of digits in the mantissa
of log n should equal the number of significant
figures in n
- In conversion to log into antilog, the number of
sig figs in antilog = number of digits in mantissa

The Real Rule

- The first digit of absolute uncertainty is the last significant digit in the answer
Lecture 6 - Statistics and Data
 Lecture 6 - Statistics and Data
Introduction to Statistics
Types of Data
- Raw Data:

- Processed Data: Data which has been subjected to any type of alteration (e.g. data
analysis, removal of outliers, removal of noise etc.)
Error Bars from Systematic Uncertainties
- Systematic Uncertainty:
- Systematic error bars
- Rarely look as systematic errors, mostly random errors, but good to check
- Systematic error is smaller than random error

Data Presentation
- PowerPoint presentation type can be hard to understand
for complex data
- Method below good (relates averages) but missing errors
Introduction to Statistic cont.
How to Find the Error of a Measurement
- Chemistry usually talks about continuous data
- Continuous vs discrete data
- Usually expect normal distribution

Normal (Gaussian) Distribution

- Statistics gives us tools to accept conclusions that have high
probability of being correct and rejecting conclusions that do not
- Also describes the variance between measurements
- If experiment repeated many times (large set of observations),
they tend to cluster in a bell-curve shape about the average value

Mean and Standard Deviation

- Mean: The sum of measured values divided by the number of
measurements
- Characteristic of Normal distributions
- Standard Deviation (s.d.): Measures how closely the data is
clustered around the mean
- Characteristic of Normal distributions
- The smaller the s.d., the more closely the data are clustered
about the mean, and the more precise the measurement is

Assessing Correlation
- First year methods learned include The Method of Least Squares, R^2 (coefficient of
determination), etc.
- These indicate the degree of correlation, but not whether one variable causes the other

Anscombe’s Quartet

- Mean of x and y, and R^2 value are the same

- R^2 doesn’t measure the goodness of fit,
predictive error, how one variable explains
another
- Statistics can be misleading:
- FILL IN
P-Hacking or Data Dredging
- p-Hacking/Data Dredging:

Cognitive Distortions in Data Analytics

- Confirmation Bias: Tendency to notice, interpret, and remember data that supports
your existing beliefs, while disregarding contradictory evidence
- Mitigation:
- e.g.
- Overconfidence Bias: Being too certain about predictions or assumptions,
underestimating uncertainty
- Mitigation:
- e.g.
- Groupthink:
- Mitigation:
- e.g.
- Availability Bias:
- Mitigation:
- e.g.

Statistical Tests
- Statistical Significance:
- PAGE 40 STUFF
- Null Hypothesis:
- Used in several tests:
- F-test:
- t-test:
Module 2
 Module 2
Liquids and their Use in
Analytical Chemistry
Lecture 7 - Acids and Bases
 Lecture 7 - Acids and Bases
Review of Chemical Equilibria
Equilibrium Constant
- The subscript c indicates that this is expressed in terms of
concentration
- Equilibrium does not depend on reaction direction at fixed
T, P
- For equilibrium to occur, neither reactants or products can
escape from the system
- Kc has no units
- Kc >> 1 - equilibrium lies to the right
- Kc << 1 - equilibrium lies to the left
- Kc = 1 - equilibrium lies to the right

Heterogenous Equilibria
- Heterogenous Equilibria: not everything is aqueous
- Concentrations of solids and pure liquids are effectively constant in heterogeneous
reaction
- Pure solids and liquids are 1 in the Kc calculations for heterogeneous reactions

Le Chatelier’s Principle
- FILL IN DEFN

Acids and Bases

- Bronsted-Lowry:
- Acid = proton donor (must have a removable proton)
- Base = proton acceptor (must have pair of non-bonding electrons)
- Can be applied to non-aqueous solutions and to gas phase
- If a molecule can be both, it is known as amphiprotic
Acids in Solution
- Acids dissociate in solution into a proton and a conjugate base
- Water acts as a Bronsted-Lowry base, forming a hydronium ion
- YOU DO NOT SEE FREE PROTONS IN SOLUTION!!!

Nomenclature
- Transformation into a conjugate involves the loss or gain of a proton
Acid and Base Strength
- Acid and Base Strength: The extent of
dissociation of the acid or base solution
- Not the same as concentration
- The scale is relative
- The conjugate base of a strong acid shows
negligible basicity
- FILL IN
- The conjugate base of a weak acid is a weak base
- FILL IN
- The conjugate base of a substance with negligible acidity is a strong base
- FILL IN

Acid/Base Behaviour as Equilibria

- FILL IN

Water Auto-Ionization
pH
- pH: Measures acidity in water
- Logarithmic scale

Dissociation Constants
- Dissociation Constant, Ka: A measure of acid
strength
- We used this since the extent of dissociation is
the prime indicator of acid strength
- The larger the Ka, the stronger the acid
Lecture 8 - Buffers and Solutions
 Lecture 8 - Buffers and Solutions
Buffers
- Buffer: A mixture of an acid and its conjugate base pair that helps a solution resists pH
change

Henderson-Hasselbach Equation

- There’s a version of the formula for pOH

What is a Solution?
- Solution: Homogenous mixture of two or more substances
- Solute: Minor species in solution
- Solvent: Major species in solution

Describing Solutions

Solution Dilution
Tab 11
 Lecture 9 - Separation Techniques
Introduction to Sample Preparation Techniques
- Goal is to get homogenous lab sample, then split into aliquots for testing

Sample Preparation
- Goal: Remove either the analyte or the interferent (something that interferes with signal or
gives it something to compete with) form the sample’s matrix
- To achieve this separation, we must identify at least one significant difference
between analyte’s and interferent’s chemical or physical properties
- Two Limiting Factors:
1. Failing to recover all the analyte
2. Failing to remove all the interferent
Separation Techniques
Module 3
Lecture 11 - Quality Assurance+Calibration
Methods
 Lecture 11 - Quality Assurance and
Calibration Methods
What is Quality Assurance?
- Quality Assurance: What we do to get the right answer
for our purpose (e.g. hypothesis) with sufficient
accuracy and precision (e.g. error analysis, stdev.) to
support subsequent decision
- “Get the right data, get the data right
(precision/accuracy), keep the data right (storage of
sample, etc.)”
- Method Validation: The process of proving that an analytical method is acceptable
for the intended purpose
- Includes determining specificity, accuracy, precision, detection limit, quantitation
limit, etc.
- Quality assurance version of "analytical chemistry”
The Quality Assurance Process

False Positives and False Negatives

- Example:

- Population = 1,000,000
 - We know that 0.4% of 1 million => will have cancer
0.4% of 1,000,000 = 4,000 have cancer X

-> How well does test Z work on the sub-population that has X?
Test: 99.5 % of 4,000 = 3,980 people have cancer X, the test is correct
0.5% of 4,000 = 20 people have cancer but the test missed them

- -> How well does the test work on the sub-population that does not have cancer
1,000,000 - 4,000 = 996,000 people are healthy
Test: 99.5% of 996,000 = 991,020 people who don’t have cancer X, test is negative -> test
works
1% of 996,000 = 9,960 people who are healthy but test positive => FALSE POSITIVE

-> Total positive tests = 3980 + 9960 = 13940

(3980/13940)*100 = 29% are TRUE positives
Other 71% are FALSE positives

- e.g. Tons of people get false positive if a cheaper test, but this allows us to narrow down
people who are true positive and specifically test them with more accuracy

Selectivity and Sensitivity

- Sensitivity: The capability of responding reliably and measurably to changes in
analyte concentration
- Specificity/Selectivity: Being able to distinguish analyte from other species in the
sample (avoiding interference)
- Detection Limit: The smallest quantity of analyte that is significant;y different from
the blank
- Must be lower than the concentrations to be measured

Blanks
- Blanks: Account for interference by other species in the sample, and for traces of
analyte found in reagents used for sample preservation, preparation and analysis
- Method Blank: A sample containing all components except the analyte and it
is taken through all the steps of the analytical procedure
- Useful for an environmental sample, where having it go through the same
procedure as the analyte heavily affects the results
 - Reagent Blank: A method blank that has not been subjected to all/any sample
preparation procedures
- Literally just the reagents
- Field Blank: A method blank that has been exposed to the site of sampling

Limit of Detection

- Detection Limit: what is told by instrument supplier

- If sample is at detection limit, ~1% of area of blank lies to the right of detection limit
(false-positives)
- 50% of the area of sample lies to the left of detection limit (false negatives)

Quantifying the Detection Limit

- “Detection limit of analyte = detection limit of blank + 3s”

 - 3s is the difference between the samples I think or something
- m is the slope of the line for the curve above
- Want to work far away from detection limit for it to be effective
- Want to work with quantitation limit for better accuracy

Calibration Curves
- Made by preparing a series of known solution of analyte
- Graph tends to be “a group of instrument response vs analyte concentration”
- External Standard: Known solutions of analyte that do not involve the unknown
- Standard Addition: Known quantities of analyte are added to the unknown
- Internal Standard: Known amount of compound (that’s different from analyte) that is
added to the unknown
Tab 15
Lecture 13 - Internal Standards
 Lecture 13 - Internal Standards
Internal Standards
Internal Standards (IS)
- FILL IN
- Internal standard questions usually have two experiments - one where we calibrate and one
where we measure

Internal Standards vs Standard Addition

- Standard error corrects for systematic errors caused by matrix
- Internal standards: random errors caused by run-to-run variation
- FILL IN

Response Factor (F)

- Standard is not the same as the analyte

- Correcting that you don’t have the same chemical compound as in the standard
Internal Standard (IS) Calibration Curves

Plotting a calibration curve using an IS

- Analyte and IS have distinct peaks at different wavelengths

- Y-axis is ratio of signals
- X-axis is ratio of analyte to IS (basically plotting amount of standard adding to each case)
- Doesn’t go thru zero visually, but doing error analysis shows it effectively goes thru zero
(within error margin or something)
Compare and Contrast (Practice Questions)

- Internal standard, internal standard

Guest Lectures
CHEM 212 Guest Lecture 1 Bingo Jobert Thornton

1. Talking about how the company makes acids (related to acids and bases unit)
2. Acidification/digestion of water staples (BL nitric and hydrochloric)
3. Primarily distilling mineral acids for trace element analysis (use acid for this)
4. Analytical Standards (calibration curve standard for manufacturing pure acids (IQ and BL)
combined with pure forms of the elements)
5. Able to trace origin of bombs with chromatography (when taking about industrial uses of the
company’s field of study/work)
6. ICP-MS (Inductively Coupled Plasma Mass Spectrometry)
7. Blanks (the zero on the calibration curve)
a. Method Blanks (all sample prep and reagents but no sample)
b. Reagent Blanks (Separate analysis of each reagent)
c. Instrument Blank
8. Digestion
a. Partial (part of the sample remains)
b. Total (all of sample decomposed)
9. Extraction (sample remains intact)
a. Analysis is method dependent (e.g. time temp, matrix)