Skip to main content

Journal articles made easy: Detecting iron

Description

This article looks at measuring iron in a variety of solutions using a scalable RGB technique. It will help you understand the research the journal article is based on, and how to read and understand journal articles. The research article was orginally published in Journal of Materials Chemistry A.

Type of Activity

:
working independently

Audience

:
TeacherStudent

Age Group

:
Undergraduate & Postgraduate
journal-articles-made-eas...

Introduction.

For each of the intermediates in the synthesis of HOxMMA, data is provided confirming the identity of the molecules.

For further information on the various spectroscopy techniques used, you can explore our Introduction to spectroscopy tool.  Here you will find an explanation of the principles for a range of spectroscopic techniques including infrared (IR), ultraviolet-visible (UV/Vis) and nuclear magnetic resonance (NMR). Each technique has a drop down box containing clear explanations and descriptions with embedded videos and clickable links to animations (many of which are interactive) to aid your learning.

In addition, our Spectraschool resource gives you the opportunity to look at and compare real spectra of compounds by zooming, overlaying them and pasting them to other documents.  There is also a problem-solving test where your mission will be to identify an unknown compound from an analysis of its spectra - a great tool to check understanding!

1H-NMR data

The 1H NMR spectra were recorded with a Varian Inova 400 spectrometer operating at 399.94 MHz for intermediate 1, or on a Varian Mercury 300 spectrometer operating at 299.87 MHz for intermediate 2 and HOxMMA. Deuterated dimethyl sulfoxide (DMSO-d6) was used as a solvent. 

Intermediate 1: 5-Chloro-7-nitroquinolin-8-ol

  • δ (ppm), 9.15 (d, 1H, 3.9 Hz); 8.67 (d, 1H, 8.4 Hz); 8.26 (s, 1H); 8.01 (dd, 1H, 8.4 and 4.4 Hz).

Intermediate 2: 7-Amino-5-chloroquinolin-8-ol

  • δ (ppm), 9.42 (s, 1H); 8.78 (d, 1H, 3.9 Hz); 8.29 (d, 1H, 8.4 Hz); 7.35 (m, 1H); 7.34 (s, 1H); 5.36 (s, 2H).

HOxMMA

  • δ (ppm), 10.72 (s, 1H); 9.32 (s, 1H); 9.00 (d, 1H, 3.9 Hz); 8.53 (d, 1H, 8.4 Hz); 8.23 (s, 1H); 7.73 (dd, 1H, 8.4 and 4.4 Hz); 5.99 (s, 1H); 5.61 (s, 1H); 2.05 (s, 3H). 

13C-NMR data

The 13C NMR spectra were recorded with a Varian Inova 400 spectrometer operating at 100.58 MHz for intermediate 1, or on a Varian Mercury 300 spectrometer operating at 75.41 MHz for intermediate 2 and HOxMMA. Deuterated dimethyl sulfoxide (DMSO-d6) was used as a solvent. 

Intermediate 1: 5-Chloro-7-nitroquinolin-8-ol

  • δ (ppm), 151.57; 150.98; 141.01; 134.59; 133.23; 129.53; 126.86; 122.99; 118.71. 

Intermediate 2: 7-Amino-5-chloroquinolin-8-ol

  • δ (ppm), 149.82; 139.39; 136.02; 135.879; 133.13; 119.96; 119.24; 118.74; 118.695.

HOxMMA

  • δ (ppm), 167.30; 150.27; 144.60; 140.56; 139.62; 133.42; 124.66; 123.99; 123.78; 123.03; 122.02; 118.85; 19.48. 

Further information on NMR spectroscopy:

Vignettes on NMR theory

Exerpt from the book 'Modern Chemical Techniques'

EI-HRMS data

High-resolution electron-impact mass spectrometry (EI-HRMS) was carried out on a Micromass AutoSpect Waters mass spectrometer (ionization energy: 70 eV; mass resolving power: >10000).

Intermediate 1: 5-Chloro-7-nitroquinolin-8-ol

  • m/z: 224 (M+, 100), 150 (90), 194 (55), 115 (46), 166 (45), 226 (35), 114 (25), 152 (21). 

Intermediate 2: 7-Amino-5-chloroquinolin-8-ol

  • m/z: 194 (M+, 100), 96 (33), 78 (22), 63 (21), 165 (15), 131 (10), 167 (9), 65 (8). 

HOxMMA

  • m/z: 262 (M+, 100), 193 (88), 41 (86), 69 (55), 165 (63), 264 (37), 195 (32), 129 (29), 221 (27). 

Further information on mass spectrometry:

Introduction to the theory of mass spectrometry.

Exceprt from the book 'Modern Chemical Techniques'

FT-IR data

Infrared spectra (FT-IR) were recorded with a Nicolet Impact spectrometer.

Intermediate 1: 5-Chloro-7-nitroquinolin-8-ol

  • FT-IR (wavenumbers, cm−1): νO–H: 2808; νAr,C[double bond, length as m-dash]C: 1600; νNO2 (as, s): 1503, 1332; νC–Cl: 1018. 

Intermediate 2: 7-Amino-5-chloroquinolin-8-ol

  • FT-IR (wavenumbers, cm−1): νC–NH2: 3320; νO–H: 3262; νAr,C[double bond, length as m-dash]C: 1588; νC–Cl: 1052. 

HOxMMA

  • FT-IR (wavenumbers, cm−1): νN–H: 3441; νO–H: 3930; νC[double bond, length as m-dash]O: 1692; νArC[double bond, length as m-dash]C: 1585; νC–Cl: 1057. 

Further information on infrared spectroscopy:

A video giving instructions on how to run an infrared spectrum.

Short screenshot videos on IR spectroscopy theory.

Introduction to the theory of IR spectroscopy.

ADDITIONAL INFORMATION

Journal articles made easy are journal articles from a range of Royal Society of Chemistry journals that have been re-written into a standard, accessible format. They contain links to the associated Chemistry World article, ChemSpider entries, related journal articles, books and Learn Chemistry resources such as videos of techniques and resources on theory and activities. They should facilitate students understanding of scientific journal articles and how to extract and interpret the information in them.