/*! This file is auto-generated */ .wp-block-button__link{color:#fff;background-color:#32373c;border-radius:9999px;box-shadow:none;text-decoration:none;padding:calc(.667em + 2px) calc(1.333em + 2px);font-size:1.125em}.wp-block-file__button{background:#32373c;color:#fff;text-decoration:none} Problem 12 Loconto and co-workers describe ... [FREE SOLUTION] | 91Ó°ÊÓ

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Loconto and co-workers describe a method for determining trace levels of water in soil. \(^{19}\) The method takes advantage of the reaction of water with calcium carbide, \(\mathrm{CaC}_{2}\), to produce acetylene gas, \(\mathrm{C}_{2} \mathrm{H}_{2}\). By carrying out the reaction in a sealed vial, the amount of acetylene produced is determined by sampling the headspace. In a typical analysis a sample of soil is placed in a sealed vial with \(\mathrm{CaC}_{2}\). Analysis of the headspace gives a blank corrected signal of \(2.70 \times 10^{5} .\) A second sample is prepared in the same manner except that a standard addition of \(5.0 \mathrm{mg} \mathrm{H}_{2} \mathrm{O} / \mathrm{g}\) soil is added, giving a blank-corrected signal of \(1.06 \times 10^{6} .\) Determine the milligrams \(\mathrm{H}_{2} \mathrm{O} / \mathrm{g}\) soil in the soil sample.

Short Answer

Expert verified
Approximately 1.71 mg \( \mathrm{H}_{2} \mathrm{O} / \mathrm{g} \) soil in the sample.

Step by step solution

01

Understand the Problem and Setup Equations

The problem involves using the method of standard additions to determine how much water is originally present in the soil sample using the reaction between water and calcium carbide to produce acetylene gas. According to the method of standard additions, the addition of a known quantity of analyte helps to determine the unknown concentration in the sample. Let the original concentration of water in the soil be \( x \) mg \( \mathrm{H}_{2} \mathrm{O} / \mathrm{g} \) soil. The signal obtained without the standard addition corresponds to \( 2.70 \times 10^5 \) and the signal with an added standard corresponds to \( 1.06 \times 10^6 \). The added standard concentration was \( 5.0 \) mg \( \mathrm{H}_{2} \mathrm{O} / \mathrm{g} \) soil.
02

Use the Method of Standard Additions Equation

For method of standard additions, the equation is:\[ \frac{S_1}{S_2} = \frac{x}{x + C_{add}} \]where \( S_1 \) is the signal from the original sample (\( 2.70 \times 10^5 \)), \( S_2 \) is the signal from the spiked sample (\( 1.06 \times 10^6 \)), \( x \) is the concentration of \( \mathrm{H}_{2} \mathrm{O} \) in the original solution, and \( C_{add} \) is the concentration of \( \mathrm{H}_{2} \mathrm{O} \) added (\( 5.0 \) mg/g).
03

Solve the Equation for x

Substitute the known values into the equation and solve for \( x \):\[ \frac{2.70 \times 10^5}{1.06 \times 10^6} = \frac{x}{x + 5.0} \]First, calculate the ratio:\[ \frac{2.70 \times 10^5}{1.06 \times 10^6} = 0.2547 \]Now solve for \( x \):\[ 0.2547(x + 5.0) = x \]\[ 0.2547x + 1.2735 = x \]Rearrange:\[ 1.2735 = x - 0.2547x \]\[ 1.2735 = 0.7453x \]Finally, solve for \( x \):\[ x = \frac{1.2735}{0.7453} \approx 1.71 \text{ mg of } \mathrm{H}_{2} \mathrm{O} / \mathrm{g} \text{ soil} \]
04

Conclusion

The concentration of water in the original soil sample is approximately \( 1.71 \) mg \( \mathrm{H}_{2} \mathrm{O} / \mathrm{g} \) soil.

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Key Concepts

These are the key concepts you need to understand to accurately answer the question.

Standard Addition Method
The Standard Addition Method is a vital analytical technique used to determine the concentration of an analyte in a complex sample. This approach is especially valuable in samples where matrix effects can modify the response by either enhancing or suppressing it. By using this method, you can correct for these effects and obtain an accurate measurement of the analyte's concentration.

In our example of determining trace water levels in soil, two main steps are typically followed in the standard addition method:
  • First, measure the response (signal) of the original sample without adding any standard. This gives the baseline reading, which in the given exercise was a signal of \(2.70 \times 10^5\).
  • Then, a known quantity of the analyte, which in this case is water, is added and the new signal is measured. This is known as the spiked sample signal, recorded as \(1.06 \times 10^6\).
By introducing a known amount of analyte, we apply the method of standard additions equation to find the unknown concentration. We determine the water concentration in soil by comparing the ratio of signals with and without the standard addition. This process eliminates the need for a calibration curve under the assumption that the background signal remains constant.
Trace Analysis
Trace Analysis is the analysis of small quantities of a substance within another material, often in parts per million (ppm) or parts per billion (ppb). In the realm of analytical chemistry, it is crucial for detecting and quantifying low levels of chemical substances. Trace analysis is essential in environmental monitoring, forensic studies, and food safety analysis, among others.

In our context, the exercise involves determining very low concentrations, or traces, of water in a soil sample. This is significant because water in soil affects many physical and chemical properties, such as nutrient availability and oxygen diffusion. The ability to accurately measure these small amounts of water is key to understanding and managing soil health and agricultural productivity.
  • Challenges: Handling trace amounts can be challenging due to contamination risks and sensitivity limits of instruments.
  • Solutions: Techniques such as the Standard Addition Method help mitigate errors due to matrix interference and improve accuracy in trace determinations.
By using the Standard Addition Method, the exercise described assesses water concentrations in soil with high accuracy and without much interference.
Headspace Analysis
Headspace Analysis is a technique used to sample the volatile substances in the gas phase above a solid or liquid sample inside a closed container. It is especially beneficial when analyzing volatile compounds as it simplifies the sample preparation process and minimizes interference from non-volatile impurities.

In the given analytical problem, headspace analysis is employed to determine the amount of acetylene gas produced by the reaction between water in the soil and calcium carbide. How does it work?
  • A sealed vial containing the soil and calcium carbide reacts to produce acetylene gas.
  • The gas enters the headspace of the vial, where its concentration is analyzed.
Using headspace analysis offers several advantages:
  • It reduces the risk of contamination since the sample remains sealed.
  • Provides rapid and simple measurement as the concentration of analytes in the headspace correlates with the concentration in the sample.
In situations where trace levels of volatile substances, such as acetylene, need to be quantified from complex matrices, headspace analysis proves to be a powerful tool.

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Most popular questions from this chapter

A mixture of \(n\) -heptane, tetrahydrofuran, 2 -butanone, and \(n\) -propanol elutes in this order when using a polar stationary phase such as Carbowax. The elution order is exactly the opposite when using a nonpolar stationary phase such as polydimethyl siloxane. Explain the order of elution in each case.

The amount of camphor in an analgesic ointment is determined by GC using the method of internal standards. \({ }^{21}\) A standard sample is prepared by placing \(45.2 \mathrm{mg}\) of camphor and \(2.00 \mathrm{~mL}\) of a \(6.00 \mathrm{mg} / \mathrm{mL}\) internal standard solution of terpene hydrate in a \(25-\mathrm{mL}\) volumetric flask and diluting to volume with \(\mathrm{CCl}_{4}\). When approximately \(2-\mu \mathrm{L}\) sample of the standard is injected, the FID signals for the two components are measured (in arbitrary units) as 67.3 for camphor and 19.8 for terpene hydrate. A 53.6-mg sample of an analgesic ointment is prepared for analysis by placing it in a \(50-\mathrm{mL}\) Erlenmeyer flask along with \(10 \mathrm{~mL}\) of \(\mathrm{CCl}_{4}\). After heating to \(50^{\circ} \mathrm{C}\) in a water bath, the sample is cooled to below room temperature and filtered. The residue is washed with two \(5-\mathrm{mL}\) portions of \(\mathrm{CCl}_{4}\) and the combined filtrates are collected in a \(25-\mathrm{mL}\) volumetric flask. After adding \(2.00 \mathrm{~mL}\) of the internal standard solution, the contents of the flask are diluted to volume with \(\mathrm{CCl}_{4}\). Analysis of an approximately \(2-\mu \mathrm{L}\) sample gives FID signals of 13.5 for the terpene hydrate and 24.9 for the camphor. Report the \(\% \mathrm{w} / \mathrm{w}\) camphor in the analgesic ointment.

Haddad and associates report the following retention factors for the reversed- phase separation of salicylamide and caffeine. \({ }^{25}\) \(\begin{array}{ccccccc}\% \text { methanol } & 30 \% & 35 \% & 40 \% & 45 \% & 50 \% & 55 \% \\ k_{\text {sal }} & 2.4 & 1.6 & 1.6 & 1.0 & 0.7 & 0.7 \\\ k_{\text {caff }} & 4.3 & 2.8 & 2.3 & 1.4 & 1.1 & 0.9\end{array}\) (a) Explain the trends in the retention factors for these compounds. (b) What is the advantage of using a mobile phase with a smaller \(\% \mathrm{v} / \mathrm{v}\) methanol? Are there any disadvantages?

The amount of caffeine in an analgesic tablet was determined by HPLC using a normal calibration curve. Standard solutions of caffeine were prepared and analyzed using a \(10-\mu L\) fixed-volume injection loop. Results for the standards are summarized in the following table. \begin{tabular}{cc} concentration \((\mathrm{ppm})\) & signal (arb. units) \\ \hline 50.0 & 8354 \\ 100.0 & 16925 \\ 150.0 & 25218 \\ 200.0 & 33584 \\ 250.0 & 42002 \end{tabular} The sample is prepared by placing a single analgesic tablet in a small beaker and adding \(10 \mathrm{~mL}\) of methanol. After allowing the sample to dissolve, the contents of the beaker, including the insoluble binder, are quantitatively transferred to a \(25-\mathrm{mL}\) volumetric flask and diluted to volume with methanol. The sample is then filtered, and a \(1.00-\mathrm{mL}\) aliquot transferred to a \(10-\mathrm{mL}\) volumetric flask and diluted to volume with methanol. When analyzed by HPLC, the signal for caffeine is found to be \(21469 .\) Report the milligrams of caffeine in the analgesic tablet.

A series of polyvinylpyridine standards of different molecular weight was analyzed by size-exclusion chromatography, yielding the following results. \begin{tabular}{cc} formula weight & retention volume (mL) \\ \hline 600000 & 6.42 \\ 100000 & 7.98 \\ 20000 & 9.30 \\ 3000 & 10.94 \end{tabular} When a preparation of polyvinylpyridine of unknown formula weight is analyzed, the retention volume is \(8.45 \mathrm{~mL}\). Report the average formula weight for the preparation.

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