Inductively coupled plasma experiments

Figures 8.14 and 8.15 from Date and Gray, Applications of Inductively Coupled Plasma Mass Spectrometry (1989) figures 2.7 and 2.8 from Kealey, Experiments in Modern Analytical Chemistry (1986) by permission of Blackie, U.K.

The samples were air-dried at room temperature, sieved to < 63 pm and analysed by x-ray diffraction (XRD) and scanning electron microscopy combined with an energy dispersive system (SEM-EDS). For chemical analysis, samples were submitted to an extraction with Aqua Regia and analysed by inductively coupled plasma-optical emission spectrometry (ICP/OES). Firing experiments were performed following the procedure described by Brindley Brown (1980). 

Wendt and Fassel [2] reported early experiments with a tear-drop shaped inductively coupled plasma but later described the medium power l-3kW 18mm annular plasma now favoured in modern analytical instruments [3]. 

In reference 190, the authors describe the spectroscopic and X-ray crystallographic techniques they used to determine the pMMO structure. First, EPR and EX AFS experiments indicated a mononuclear, type 2 Cu(II) center hgated by histidine residues and a copper-containing cluster characterized by a 2.57 A Cu-Cu interaction. A functional iron center was also indicated by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES). ICP-AES uses inductively coupled plasma to produce excited atoms that emit electromagnetic radiation at a wavelength characteristic of a particular element. The intensity of this emission is indicative of the concentration of the element (iron in this case) within the sample. 

Chemically pure reagents were used. Cadmium was added as its sulfate salt in concentrations of about 50 ppm. Lanthanides were added as nitrates. For the experiments with other metal ions so-called "black acid from a Nissan-H process was used. In this acid a large number of metal ions were present. To achieve calcium sulfate precipitation two solutions, one consisting of calcium phosphate in phosphoric acid and the other of a phosphoric acid/sulfuric acid mixture, were fed simultaneously in the 1 liter MSMPR crystallizer. The power input by the turbine stirrer was 1 kW/m. The solid content was about 10%. Each experiment was conducted for at least 8 residence times to obtain a steady state. During the experiments lic iid and solid samples were taken for analysis by ICP (Inductively Coupled Plasma spectrometry, based on atomic emission) and/or INAA (Instrumental Neutron Activation Analysis). The solid samples were washed with saturated gypsum solution (3x) and with acetone (3x), and subsequently dried at 30 C. The details of the continuous crystallization experiments are given in ref. [5]. 

Vanderpool, R.A., D. Hoff, and PE. Johnson. 1994. Use of inductively coupled plasma-mass spectrometry in boron-10 stable isotope experiments with plants, rats, and animals. Environ. Health Perspec. 102(Suppl. 7) 13-20. 

In addition to these, there were experiments exploiting quartz crystal microbalances (55), matrix isolation (86), differential scanning calorimetry (87), capillary electrophoresis (88), and inductively coupled plasma (1CP) spectrometers (89). 

Fourier transform ICR mass spectrometers together with any type of ion source, such as nanoESI, MALDI (or also an inductively coupled plasma ion source) permit mass spectrometric measurements to be performed at ultrahigh mass resolution (R = m/hm = 105—106) with a very low detection limit and the highest possible mass accuracy (Am = 10 3—10 4 Da). In addition, a high mass range is possible and FTICR-MS can be applied for MS/MS experiments.48 A comparison of different separation systems used in inorganic mass spectrometry is presented in Table 3.1. 

Several other microanalytical methods in common use potentially have application on soil and sediments section samples. Laser-ablation inductively coupled plasma mass spectrometery (LA-ICP-MS) has been used on soil thin-sections from a controlled field experiment (21) but required special resins in the preparation. There is presently (May 2006) no reported use of this method on archaeological soil samples. Likewise, for extremely fine-resolution studies (i.e. <10 pm) with low minimum detection limits and despite difficult calibration, secondary ion microscopy (SIMS) has a potential role in examining archaeological soil thin sections. At even higher lateral resolutions ( 100 nm) Auger electron spectroscopy (AES) could also be considered for surface (<5 nm deep) analyses. At present however, the use of these methods in soil systems is limited. SIMS has been focused on biochemical applications (22), whereas AES... 

This experiment presents the measurement of uranium with an inductively coupled plasma mass spectrometer (ICP-MS). In this system, a nebulizer converts the aqueous sample to an aerosol carried with argon gas. A torch heats the aerosol to vaporize and atomize the contents in quartz tubes. The atoms are ionized with an efficiency of about 95% by an RF (radiofrequency) coil. The plasma expands at a differentially-pumped air-vacuum interface into a vacuum chamber. The positive ions are focused and injected into the MS while the rest of the gas is removed by the pump. The ions are then accelerated, collected, and measured as a function of their mass. Losses at various stages, notably the vacuum interface, result in a detection efficiency of about 0.1 %, which is still sufficient to provide great sensitivity. The amounts of uranium isotopes in the sample are determined by comparisons to standards. Because different laboratories have different instruments, the instructor will provide instrument operating instmctions. Do not use the instrument until the instructor has checked the instrument and approved its use. 

Contamination of the analytes from the carriers (the precipitates) should be first examined, and the blank test carried out carefully. Great care should also be taken in terms of the recoveries of the analytes, because the procedures in the coprecipitation are sometimes time-consuming and irre-producible. Some efficiencies of recovery for Zr(IV) coprecipitation along with the determined values of trace elements in seawater are summarized in Table 7, where inductively-coupled plasma (ICP) emission spectrometry was applied for the simultaneous multielement analysis [45]. In this experiment, 10 mg of Zr(IV) was added to 11 of seawater, the precipitation made... 

---