Additive analysis Inductively coupled atomic emission

The analytical techniques used for additives analysis are reviewed below. They are mainly chromatographic but enzymatic, flow injection analysis, inductively coupled plasma-atomic emission spectrometry and atomic absorption methods are also used. 

In addition to the cation used to prepare the polymer, other cations with differing charges, sizes, coordination numbers and/or coordination geometries are used in these selectivity quotient measurements to verify specificity. Measurements are also made using polymers prepared with no metal cation (H or NH4 ) as experimental controls. The measurements required for these studies are made using a pH meter for [H ] and elemental analysis (inductively coupled plasma atomic emission spectrometry (ICP-AES) or inductively coupled plasma mass spectrometry (ICP-MS))for [M"-"]. 

The objective of this symposium and this book is to acquaint the readers with the latest advances in the field of elemental analysis and to focus on what avenues of future research to explore in this area. The subjects included are various elemental analysis techniques such as atomic absorption spectrometry, inductively coupled plasma emission and mass spectrometry, isotope dilution mass spectrometry. X-ray fluorescence, ion chromatography, gas chromatography-atomic emission detection, other hyphenated techniques, hetero-atom microanalysis, sample preparation, reference materials, and other subjects related to matrices such as petroleum products, lubricating oils and additives, crude oils, used oils, catalysts, etc. 

Produced HBr is scrubbed by the use of 10 N sodium hydroxide solution to form sodium bromide. For all the runs, the initial inventory is 1.25 L of sodium hydroxide solution. The NaOH solution was sampled at regular intervals and sent to Argonne s Analytical Chemistry Laboratory for analysis. Volume aliquots of solution samples were diluted with reagent water and analysed by ion chromatography to determine bromide. Separate aliquots were diluted with acid addition and analysed by inductively coupled plasma-atomic emission spectrometry (ICP-AES) to determine calcium. During the data analysis, adjustments are made for the addition of condensed unreacted steam to the neutralisation solution. 

Multielement analysis will become more important in industrial hygiene analysis as the number of elements per sample and the numbers of samples increases. Additional requirements that will push development of atomic absorption techniques and may encourage the use of new techniques are lower detction and sample speciation. Sample speciation will probably require the use of a chromatographic technique coupled to the spectroscopic instrumentation as an elemental detector. This type of instrumental marriage will not be seen in routine analysis. The use of Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) (17), Zeeman-effect atomic absorption spectroscopy (ZAA) (18), and X-ray fluorescence (XRF) (19) will increase in industrial hygiene laboratories because they each offer advantages or detection that AAS does not. 

Hydrous sodium titanate was prepared by the method of Dosch and Stephens (1). Titanium isopropoxide was slowly added to a 15 wt% solution of sodium hydroxide in methanol. The resulting solution was hydrolyzed by addition to 10 vol% water in acetone. The hydrolysis product is an amorphous hydrous oxide with a Na Ti ratio of 0.5 which contains, after vacuum drying at room temperature, approximately 13.5 wt% water and 2.5 wt% residual alcohol. The ion-exchange characteristics of the sodium titanate and the hydrolysis behavior of the nickel nitrate solutions were characterized using a combination of potentiometric titrations, inductively coupled plasma atomic emission (ICP) analysis of filtrates, and surface charge measurements obtained using a Matec electrosonic amplitude device. 

Phosphorus can serve as a benehcial adjunct or as a deleterious agent. There are several test methods for the determination of phosphorus. In addition to the three test methods described here, reference should also be made to multielement analysis methods such as inductively coupled plasma atomic emission spectroscopy (ICPAES) (ASTM D-4951, ASTM D-5185) and X-ray fluorescence (XRF) (ASTM D-4927, ASTM D-6443) described above in this guide. Phosphorus can also be determined by a photometric procedure (IP 148) or by a test method (ASTM D-1091) in which the organic material in the sample is destroyed, phosphorus in the sample is converted to phosphate ion by oxidation with sulfuric acid, nitric acid, and hydrogen peroxide, and the magnesium pyrophosphate is determined gravimetrically. Another method (ASTM D-4047, IP 149) in which the phosphorus is converted to quinoline phosphomolybdate is also available. 

B.F. Reis, M.F. Cine, F.J. Krug, H. Bergamin-Filho, Multipurpose flow-injection system. Part 1. Programmable dilutions and standard additions for plant digests analysis by inductively coupled plasma atomic emission spectrometry, J. Anal. At. Spectrom. 7 (1992) 865. 

Y. Israel and R. M. Barnes, Standard Addition Method in Flow Injection Analysis with Inductively Coupled Plasma Atomic Emission Spectrometry. Anal. Chem., 56 (1984) 1188. 

An EPA-approved procedure for the analysis of plutonium in water is listed in Table 6-2. In addition, the following ASTM standard methods relate to the measurement of plutonium in water D 3648, D 3084, D 3972, and D 1943 (ASTM 1981, 1982a, 1982b, 1987). Recent work has focused on more rapid analytical methods in order to determine monitor plutonium levels in waste process streams at nuclear facilities. For example, Edelson et al. (1986) have investigated the applications of inductively-coupled plasma-atomic emission spectrometry (ICP-EAS) to routinely analyze water samples. 

Although originally FIA was conceived as a special technique for delivery of a sample segment into the instrument, the combination of flow injection as a sample pretreatment tool with atomic spectrometry has been shown to be of great potential for enhancing the selectivity and sensitivity of the measurements. Moreover, contamination problems are reduced due to the closed system used, making this interface suitable for ultratrace determination of metal species. Hyphenated techniques such as FIA/ SIA with flame atomic absorption spectrometry, inductively coupled plasma (ICP)-optical emission spectrometry, and ICP-mass spectrometry (MS) have been exploited extensively in recent years. The major attraction of FIA-ICP-MS is its exceptional multi-elemental sensitivity combined with high speed of analysis. In addition, the possibility of... 

Atomic absorption spectrometry (both using flame and electrothermal atomization) and plasma emission spectrometry, especially inductively coupled plasma-atomic emission spectrometry (ICP-AES) provide selective methods for quantification of inorganic species at different concentrations. These techniques are important for the analysis of inorganic pigments, charges (especially inorganic extenders), and additives such as catalysts, driers, and antifouling compovmds. 

LiBOi can be carried out in a platinum crucible at 1000°C. Acid digestion typically involves acid mixtures such as concentrated nitric and hydrochloric acid heated to temperatures of 100°C or more. The aim of the digestion in this case is to completely break down the matrix. Total tin analysis is routinely carried out using atomic absorption spectrometry (AAS) and inductively coupled plasma (ICP) coupled with atomic emission spectrometry (AES) or with mass spectrometry (MS). Hydride generation is commonly used to reduce detection limits. This technique involves the addition of a reductant such as sodium borohydride to form tin hydride. Hydride generation has been used commonly with ICP-AES, ICP-MS, and AAS. Other techniques employed for total tin determination are instrumental neutron activation and X-ray fluorescence spectrometry. 

The inductively coupled plasma (ICP) atomic emission spectrometer (AES) is used for the high-sensitivity detection of metals in dissolved samples. Applications include metals analysis of polymers, additives, catalysts, and other components on polymers and plastic formulations as well as advanced composite materials. The operating principle is essentially the same as in ICP-MS, instrument with the main difference being the detector. While the ICP-MS detector is a quadruple mass spectrometer which detects elements by their mass, the ICP-AES uses a detector based on the specific energy frequency emitted by each element in the plasma. 

Atomic absorption remains a staple of forensic chemistry, given its low cost, simple operation, and easy maintenance. The limitations are related to versatility. Unless multielement lamps are used, only one element can be tested for at a time, and each element requires a separate lamp and instrument optimization. For small target lists such as a list of barium, antimony, and lead for GSR, this is not onerous, but still is inconvenient. Limits of detection are in the low-ppm to high-ppb range for most elements, As a result, a few forensic laboratories have turned to inductively coupled plasma atomic emission spectroscopy (ICP-AES) for additional elemental analysis capability. 

As in inductively coupled plasma optical emission (ICP-OES) spectra, in addition to atomic lines, intense ionic lines are also observed, the use of an ICP as an ion source for MS seemed logical, but overcoming the difference in pressure between the ICP (generated at atmospheric pressure) and the mass spectrometer (10 —10 mbar) proved difficult and had to be accomplished via the use of a two-cone interface. Despite the advantages that double-focusing sector field mass spectrometers (higher mass resolution) and TOP analyzers (high data acquisition speed) can offer, approximately 90% of the ICP-MS units used worldwide are equipped with a quadrupole filter for mass analysis. 

A recent review by Balaram gives an account of the various instrumental techniques used in geological analysis. These include atomic absorption spectroscopy and inductively coupled plasma atomic emission spectroscopy as well as X-ray fluorescence, isotope dilution mass spectrometry and neutron activation analysis in addition to recent developments in inductively coupled plasma mass spectrometry especially in rare earth element analysis. 

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