Calculating Recovery
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Understanding Surrogates
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Welcome everyone! Today, we will explore what a surrogate is. Can someone tell me why we might use one?
Isn't it because it behaves like the analyte we're interested in?
Exactly! A surrogate mimics the analyte's properties during the extraction. It allows us to estimate how much analyte we can expect to recover.
What if the surrogate doesn’t behave like the analyte?
Good question! If the surrogate's behavior deviates from that of the analyte, our recovery calculations can be misleading, leading to inaccuracies.
Remember the acronym SURE: Surrogate Utilized for Recovery Estimation. It helps you remember the main purpose of a surrogate!
Nice mnemonic! Can we continue with the example?
Extraction Procedure
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Next, let’s talk about the extraction process. We add 50 ml of hexane to our sample to extract the surrogate. Why do we use hexane?
Hexane is a nonpolar solvent, right? It helps extract nonpolar compounds.
Exactly! And after shaking, we take out 40 ml for analysis. Can anyone explain why we don’t take all 50 ml?
Some of the hexane might not separate properly, right?
Yes, it’s often because of the difficulty in separating phases. Good point! So, fingering finger for those small residual amounts can impact our recovery rates.
Now, who remembers the efficiency of extraction we discussed previously? Connect that to the extraction process.
It affects how much of the analyte and surrogate we recover, right?
Concentration and Calibration
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Now, let’s focus on why we concentrate our samples. Why do we reduce the volume from 40 ml to 1 ml?
To increase the concentration for better detection in the instrument!
Precisely! By concentrating the sample, you're minimizing the volume and maximizing the chance of detecting lower concentrations of the analyte.
And then we calibrate the instrument with known values, right?
Absolutely! Calibration ensures we can interpret the responses from our analyses accurately. If we get an instrument response of 80,000 units, how do we relate that to the mass of the analyte?
We use the calibration equation to find the mass!
Great! And keep in mind the formula: Response = 60000 * mass – it’ll help you connect the dots.
Back Calculating Recovery
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Finally, we need to back calculate to find out how much analyte we recovered based on the surrogate response. If our instrument gave us a total of 1.3 nanograms in our 1 ml sample, how do we find the recovery?
We need to compare that to the original amount we added, right?
Exactly! So if we added 100 micrograms, how does that relate?
We find the percentage recovery by comparing the recovered mass to what we initially added.
Correct! It’s crucial to perform these calculations accurately to interpret the efficacy of the extraction and the analysis.
Could errors in our calculations affect our results?
Absolutely! Always check your units and ensure accuracy. Accuracy is key in reporting what you find.
Introduction & Overview
Read summaries of the section's main ideas at different levels of detail.
Quick Overview
Standard
In this section, the process of calculating the recovery of an analyte of interest in a sample using a surrogate compound is outlined. It illustrates the methodology by detailing the extraction steps, volume and concentration adjustments, and how to use calibration data to determine the mass of the analyte based on instrument response.
Detailed
Detailed Summary
This section focuses on Calculating Recovery of an analyte using a surrogate compound, a critical aspect of quantitative analysis in environmental chemistry. The surrogate is a known compound that behaves similarly to the analyte in the extraction process, allowing analysts to estimate how much of the analyte was recovered during analysis.
Key Points Discussed:
- Definition of Surrogates: The section opens by defining a surrogate and its role in analytical chemistry, emphasizing its similarity to the analyte of interest, which aids in identifying recovery rates.
- Mass Calculation of the Surrogate: A specific example employing a 1-liter sample with a 1 ml addition of a 100 mg/L surrogate solution is provided. The amount added is calculated as 0.1 mg, which sets the groundwork for recovery calculations.
- Extraction Process: The extraction method is explained in depth; 50 ml of hexane is added to the sample. The process includes discussing liquid-liquid extraction techniques and the practicalities of sample handling.
- Concentration Steps: After extraction, the hexane layer containing the surrogate is reduced to 1 ml for analysis to improve the detection capability. The necessity of concentration is explained concerning enhancing instrument response.
- Calibration and Response: A critical formula for calculating the mass based on calibration response is shared (60,000 times the mass of analyte). The calculated response from an instrument (80,000 units) correlates to an estimated mass leading toward determining recovery rates.
- Back Calculations for Recovery: The section describes back-calculating to determine how much surrogate was initially in the sample before analysis, emphasizing the importance of accounting for recovery rates to estimate the analyte concentration accurately.
- Common Errors: It stresses the importance of unit conversions and the potential errors that may arise during calculations, providing insights into maintaining accuracy during analysis.
- Recovery Indicators: The final parts discuss how surrogate recovery corresponds to the analyte and the complexities of solid and liquid sample recoveries, including challenges of extraction efficiencies.
Audio Book
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Introduction to Surrogates
Chapter 1 of 7
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Chapter Content
SoproblemCrelatesto,youhaveasample,1liter.Tothis,weareadding1mlof100milligrams solution of a surrogate. So, on Friday's class we discussed what a surrogate is? The surrogate is a compound that likely to behave like the analyte of interest. So A is analyte of interest that we are interested in finding concentration of. We are calculating the recovery of A in the process of analysis, so the surrogate is expected to behave like the main compound and we calculatetheefficiency ofrecovery ofAby using the efficiency ofrecovery ofthe surrogate.
Detailed Explanation
This chunk introduces the concept of surrogates in environmental analysis. A surrogate is a substance used in experiments to mimic the behavior of the analyte (the substance we are trying to measure) under investigation. Here, you start with a sample of 1 liter and add 1 mL of a surrogate solution that contains 100 milligrams of the surrogate compound. The purpose of using a surrogate is to indirectly measure the concentration of the analyte by calculating how much of the surrogate is recovered during the analysis. This allows us to understand the efficiency of the recovery process for the analyte as well.
Examples & Analogies
Consider a chef who wants to know how well a dish tastes, but instead of using the special ingredient, they use something similar like a common spice. By using the common spice (the surrogate), the chef can estimate how well the dish will do with the special ingredient. The tasting feedback they get from the common spice can help predict the overall success of the dish when the special ingredient is eventually used.
Extraction Procedure
Chapter 2 of 7
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Chapter Content
Sointhisproblemweadd1mlof100milligramsperliter.Sohowmuchwhatweareadding? Themassofsurrogatethatweareadding,addedis100milligramsperliterinto1mlthatis10 raised to -3 liters that is 0.1 milligram, this is what you are adding. We find the recovery by finding out how much of this is recovered in the end by the instrument eventually and based on that we figure out how much is lost.
Detailed Explanation
This chunk explains how to quantify the amount of surrogate being added. We're adding 1 mL from a 100 mg/L solution, which means the mass of the surrogate added is 0.1 milligrams (since 1 mL equals 10^-3 liters). To calculate the recovery of analyte A, we eventually determine how much of the surrogate was retrieved in the analysis. Comparing the initial amount of the surrogate to the amount recovered helps to figure out how much was lost during the process, thereby reflecting how much of analyte A might be potentially lost as well.
Examples & Analogies
Imagine you have a glass of juice, and you add a few drops of food coloring (the surrogate) to it. If after some time, you fill a small cup with the colored juice and measure how much color remains versus how much was originally in the glass, you can determine how well the food coloring spread through the juice. The amount you can retrieve gives you an idea of how effective the mixing (recovery) has been.
Understanding Liquid-Liquid Extraction
Chapter 3 of 7
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Chapter Content
So the problem gives you the extraction procedure. The sample was extracted with 50 ml of hexane okay. So 50 ml of hexane was added okay. So right now we are not looking at A, we are only looking at a surrogate. We are using the surrogate analysis only in this, but we can also be lookingat Ain this process, so the calculation isthe same ifweare doing.
Detailed Explanation
Here, we discuss the liquid-liquid extraction process using hexane, which is an organic solvent. The sample containing the surrogate is mixed with 50 mL of hexane to facilitate extraction. In this step, we focus solely on the surrogate recovery, but the same principles would apply if we were measuring the analyte A as well. Hexane is used to extract the surrogate from the aqueous phase, as organic solvents are typically effective at dissolving many organic compounds, allowing them to be pulled from the water and into the hexane layer.
Examples & Analogies
Think of how oil and water don’t mix. If you had a salad dressing with oil (hexane) on top of your water (sample), the oil would rise above the water. If you tried to extract just the flavoring from the water using the oil, you would shake the container and see how the flavor moves into the oil layer. This is similar to how hexane pulls organic compounds from the water sample.
Concentration Step
Chapter 4 of 7
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Chapter Content
Now this, we further process it. Sointheexamplewhatwehaveseenisthisextractwasfurtherconcentratedto1ml. Sotypicallyconcentration of this was very small volume. Weareconcentrating40mlto1ml.
Detailed Explanation
After extracting with the hexane, the next step is concentration. The entire 40 mL of hexane extract is reduced to 1 mL. This concentration process is crucial for increasing the chances of detecting the analyte or surrogate in subsequent analysis. Instruments often work better with smaller sample sizes of concentrated solutions, making detection of trace analytes much easier. Various equipment, like rotary evaporators or gentle nitrogen flows, can be employed to remove the solvent effectively.
Examples & Analogies
Consider making a concentrated soup from a larger pot of broth. By boiling down the liquid and reducing it to just a small cup of concentrated soup, the flavors become stronger and more pronounced. Just like in our laboratory, the concentrated broth (the extract) enhances the ability to taste (detect) the flavors.
Calibration and Response Calculation
Chapter 5 of 7
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Chapter Content
We will go to the next page. The response here says calibration and its response = 60,000×m, m is mass of the analyte in nanograms and the instrument response was obtained to be 80,000 units.
Detailed Explanation
Calibration is the process of establishing a relationship between an instrument’s response and the concentration of a substance. The provided equation indicates that the instrument produces a response proportional to the mass of the analyte. With a response of 80,000 units measured for the surrogate, we can calculate the mass of the surrogate in nanograms by rearranging the calibration equation (mass = response/60,000). This gives us the mass needed for further calculations based on the concentration of the sampled extract.
Examples & Analogies
Imagine you have a scale that measures how much something weighs in kilos, but all you have is a common object like a 1-kg weight to compare against. As you determine the response on the scale for various weights, you create a calibration that allows you to weigh anything accurately. Similarly, in our lab, we use known values to understand and measure unknown ones.
Back Calculation for Recovery
Chapter 6 of 7
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Chapter Content
So we are interested in finding out how much of it is that being extracted into this particular level? So you are backcalculating until this point and then we will then compare it with whatever we added okay.
Detailed Explanation
This chunk details the back calculation step, where we must find out how much of the surrogate was effectively recovered after it was analyzed. By comparing the mass of the surrogate expected based on initial conditions to what was actually recovered, we can determine the recovery efficiency. In this analysis, if 167 ng were recovered from the expected 100 ng added, it indicates a problem, prompting further examination into errors in measurement or calibration.
Examples & Analogies
Think of a treasure map where you expected to find a certain amount of gold coins buried, but upon digging, you find more or less than what you anticipated. You then have to calculate where you went wrong—if the map was accurate or if you lost some coins along the way. This backtracking allows you to assess the reliability of your marked treasure spots.
Potential Errors and Importance of Accuracy
Chapter 7 of 7
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Chapter Content
So normally you would see if there are only losses occurring, you will see this number is usually lower than this number okay, but since we are doing this, something is wrong somewhere, either the calibration is wrong or the mass that we have calculated is wrong.
Detailed Explanation
This section cautions about the common pitfalls in the calculation process. If a recovery value significantly exceeds the amount originally added, it indicates errors either in calibration or measurement. Accurate mass assessment through rigorous techniques is crucial; otherwise, one may arrive at incorrect conclusions about analyte recovery. Identifying and addressing these errors is a fundamental part of analytical chemistry to ensure reliable results.
Examples & Analogies
Imagine a baker expecting to use a specific amount of flour but ends up with a lot more after baking. It signals that either the recipe or measurements were incorrect, leading to a cake that's not what was intended. Identifying these mistakes is vital in both baking and analytical chemistry.
Key Concepts
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Surrogates: Compounds used to mimic analytes for accurate recovery calculations.
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Extraction Process: The method employed to isolate compounds from a sample.
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Concentration Steps: Reducing sample volume to enhance detection of target analytes.
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Calibration: The process of setting instrument parameters to ensure accurate measurements.
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Recovery Rate: A key metric that indicates the effectiveness of the analytical process.
Examples & Applications
In a study where a surrogate is added to a water sample, if the original concentration is 100 micrograms and the instrument returns a recovery of 70 micrograms, the recovery rate is 70%.
For soil samples, after extraction and analysis, if it is determined that 50 nanograms of an analyte are recovered from a 100 nanograms sample added, the recovery rate would be 50%.
Memory Aids
Interactive tools to help you remember key concepts
Rhymes
For surrogates, it's really quite clever, they mimic analytes, helping us measure!
Stories
Imagine a detective (the surrogate) following a suspect (the analyte) to understand the case (the recovery process) better. The detective's journey shares insight into how much the suspect behaves in various situations.
Memory Tools
M.A.R.C.: Measure - Analyze - Recover - Calculate, steps to follow during recovery analysis.
Acronyms
SURE
Surrogate Utilized for Recovery Estimation.
Flash Cards
Glossary
- Surrogate
A compound added to a sample that behaves similarly to the analyte of interest and is used to estimate recovery rates.
- Extraction
The process of separating a substance from a mixture, typically done to isolate specific compounds for analysis.
- Concentration
The process of reducing the volume of a solution to increase the amount of solute per unit volume.
- Calibration
The process of adjusting the instrument's response based on known concentrations of a standard to ensure accurate results.
- Recovery Rate
The percentage of an analyte that is recovered during the analytical process, compared to the amount that was originally present.
Reference links
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