Phosphorus inductively coupled plasma

The section on Spectroscopy has been retained but with some revisions and expansion. The section includes ultraviolet-visible spectroscopy, fluorescence, infrared and Raman spectroscopy, and X-ray spectrometry. Detection limits are listed for the elements when using flame emission, flame atomic absorption, electrothermal atomic absorption, argon induction coupled plasma, and flame atomic fluorescence. Nuclear magnetic resonance embraces tables for the nuclear properties of the elements, proton chemical shifts and coupling constants, and similar material for carbon-13, boron-11, nitrogen-15, fluorine-19, silicon-19, and phosphorus-31. 

Bednar AJ, Mirecki JE, Inouye LS, Winfield LE, Larson SL, Ringelberg DB. The determination of tungsten, molybdenum, and phosphorus oxyanions by high performance liquid chromatography inductively coupled plasma mass spectrometry. Talanta 2007 72 1828-1832. 

It is seen by examination of Table 1.11(b) that a wide variety of techniques have been employed including spectrophotometry (four determinants), combustion and wet digestion methods and inductively coupled plasma atomic emission spectrometry (three determinants each), atomic absorption spectrometry, potentiometric methods, molecular absorption spectrometry and gas chromatography (two determinants each), and flow-injection analysis and neutron activation analysis (one determinant each). Between them these techniques are capable of determining boron, halogens, total and particulate carbon, nitrogen, phosphorus, sulphur, silicon, selenium, arsenic antimony and bismuth in soils. 

Atomic absorption spectrometric methods and, more recently, the inductively coupled plasma atomic emission method, are, of course, mandatory if determination of elements is required (arsenic, selenium, boron, phosphorus and silicon). 

Que Hee and Boyle [70] analysed soils for total phosphorus using Parr bomb digestion with hydrofluoric-nitric-perchloric acids followed by inductively coupled plasma atomic emission spectrometry. 

The rhodium catalyst was recycled batch-wise four times. It was found that a short induction period occurred during the first reaction cycle. The following cycles showed a constant rate and no loss of activity was detected. A ligand-to-rhodium ratio of 5 1 led to a constant yield of 95% per cycle after 1 h. Within the four cycles a total turnover number of 1000 with a maximum turnover frequency of 234 h was achieved. The leaching of rhodium and phosphorus into the aqueous layer was determined by inductively coupled plasma atomic emission spectrometry. Rhodium leaching amounted to 14.2 ppm in the first run, then dropped to 3.6 ppm (second run) and reached values of 0.95 and 0.63 ppm in the third and fourth runs, respectively. 

A. P. Krushevska, K. Klimash, J. F. Smith, E. A. Williams, P. J. McCloskey and V. Ravikumar, Determination of phosphorus in polymeric systems using an ashing procedure and inductively coupled plasma atomic emission spectrometry, J. Anal. At. Spectrom., 19(9), 2004, 1186-1191. 

A number of instrumental analytical techniques can be used to measure the total phosphorus content of organophosphorus compounds, regardless of the chemical bonding of phosphorus within the molecules, as opposed to the determination of phosphate in mineralized samples. If the substances are soluble, there is no need for their destruction and for the conversion of phosphorus into phosphate, a considerable advantage over chemical procedures. The most important methods are flame photometry and inductively coupled plasma atomic emission spectrometry the previously described atomic absorption spectrometry is sometimes useful. 

Oxygen and nitrogen also are determined by conductivity or chromatographic techniques following a hot vacuum extraction or inert-gas fusion of hafnium with a noble metal (25,26). Nitrogen also may be determined by the Kjeldahl technique (19). Phosphorus is determined by phosphine evolution and flame-emission detection. Chloride is determined indirecdy by atomic absorption or x-ray spectroscopy, or at higher levels by a selective-ion electrode. Fluoride can be determined similarly (27,28). Uranium and U-235 have been determined by inductively coupled plasma mass spectroscopy (29). 

Analysis of major elements (except Si) and total phosphorus on bomb-digested samples was accomplished by inductively coupled plasma emission spectrometry (ICP, ARL model 34,000). Silicon was analyzed colorimetrically (14). Phosphorus in total digests was also determined colorimetrically by the method of Murphy and Riley (15), as modified by Erickson (16). To avoid interference from fluoride ion used in the digestion technique, sample volumes were restricted to <1.5 mL in the standard P analytical protocol. 

Peroxide Value, Fats and Oils (PV) (Cd 8-53) determines all substances, in terms of milliequivalents of peroxide per 1000 g of sample, that oxidize potassium iodide (KI). These substances generally are assumed to be peroxides or products of fat oxidation. Phosphorus in Oils (Ca 13-55) estimates the phospholipid content of crude, degummed, and refined vegetable oils in terms of phosphorus. Refineries often use induction coupled plasma (ICP) spectrographs to analyze divalent cations rapidly in aspirated crude oil. The calcium and magnesium measured are mainly responsible for nonhydratable phosphatides (NHP) and are determined directly. An AOCS method for analysis by ICP is being developed. 

A combination of IPC and inductively coupled plasma (ICP) MS was extensively explored for the speciation of phosphorus, arsenic, selenium, cadmium, mercury, and chromium compounds [108-118] because it provides specific and sensitive element detection. Selenium IPC speciation was joined to atomic fluorescent spectrometry via an interface in which all selenium species were reduced by thiourea before conventional hydride generation [119], Coupling IPC separation of monomethyl and mercuric Hg in biotic samples by formation of their thiourea complexes with cold vapor generation and atomic fluorescence detection was successfully validated [120]. The coupling of IPC with atomic absorption spectrometry was also used for online speciation of Cr(III) and Cr(VI) [121] and arsenic compounds employing hydride generation [122]. 

Official Methods of Analysis of AOAC International, 17th edn. Rev 1, AOAC International, Gaithersburg, MD, USA, Official Method 984.27. Calcium, Copper, Iron, Magnesium, Manganese, Phosphorus, Potassium, Sodium, and Zinc in Infant Formula - Inductively Coupled Plasma Emission Spectroscopic Method (2002)... 

International Organization for Standardization ISO 10540-3, Animal and Vegetable Fats and Oils - Determination of Phosphorus Content - Part 3 Method Using Inductively Coupled Plasma (ICP) Optical Emission Spectroscopy (2002)... 

This chapter discusses the advantages and limitations of the multielement analysis of biologically related samples using induction-coupled plasma optical emission. The sample categories covered include grains, feeds, fish, bovine liver, orchard leaves, and human kidney stones. These materials have been simultaneously analyzed for copper, nickel, vanadium, chromium, phosphorus, cobalt, lead, potassium, zinc, manganese, iron, strontium, sodium, aluminum, calcium, magnesium, silicon, boron, and beryllium, often with limited amounts of sample. 

An ultrasonic nebulizer has been designed and used for inductively coupled plasma atomic emission spectrometry [60] and microwave induced plasma-atomic emission spectrometry [61]. The apparatus is inexpensive and can be operated conveniently. Using this nebulizer, the detection limits of many elements, such as phosphorus, aluminum, and silver, were much reduced compared with the limits obtained using an aerodynamic nebulizer [62-64], The ultrasonic nebulizer was found to be suitable for samples which have a high salt concentration. 

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. 

Precursors and catalysts were characterized in ambient conditions by X-ray diffraction (XRD) on a Rigaku Powder Diffractometer using CuK radiation with a Ni filter. LiF was used as an internal standard for the activated catalysts. Laser Raman spectra (LRS) were collected using Ar ion laser excitation (514.5 nm) at a power of 25 mW at the sample. Spectra for the precursors were collected in ambient conditions, and reaction-used catalysts were characterized in-situ at 400°C in a 70 ml/min flow of C4H,(/02/He (0.99/10.2/88.81). Phosphorus to vanadium ratios (molar) were determined by inductively coupled plasma (ICP). Diffuse reflectance spectra (DRS) were collected in ambient conditions using polytetrafluoroethylene as a reference. 

Characterisation methods. Vanadium and phosphorus contents were determined by an ICP analysis (inductive coupled plasma atomic absorption) after dissolution in 0.1 M nitric acid, carbon by measuring the amount of CO2 produced by total oxidation using Coulomat 702 Stroelheim. The BET specific surface area was obtained using ASPAP 2000 (Micromeritics) by nitrogen adsorption at - 196 °C after degassing samples at 125 °C. 

Heavy metals, boron (B(V)), arsenic and total phosphorus were determined in the fraction < 20 pm to improve the comparability of the results. This fraction was separated from the freeze-dried and non-milled samples by ultrasonic sieving (Ackermann 1980). Metals were analysed after microwave-assisted digestion with aqua regia at 180 °C in closed vessels by inductively coupled plasma optical emission spectroscopy, atomic fluorescence spectroscopy (mercury) and hydride atomic absorption spectroscopy (arsenic). 

The ASTM F 1185 designation specifies chemical and crystallographic requirements for hydroxyapatite applied to the surfaces of surgical implants. Elemental analyses for calcium and phosphorus will confirm the expected stoichiometry of hydroxyapatite. The calcium and phosphorus contents will be determined by a suitable method such as ion chromatography. A quantitative X-ray diffraction analysis will determine a hydroxyapatite content of at least 95%. The concentration of deleterious trace elements such as arsenic, cadmium, mercury and lead will be assessed for hydroxyapatite derived from natural resources. The analysis of other trace elements may be required, based on the conditions, apparatus or environments specific to the manufacturing techniques and raw materials. Inductively coupled plasma/mass spectroscopy (ICP/MS), atomic absorption (AAS) or the... 

Elemental Analyses—A Leeman Model PS 1000 inductively coupled plasma (ICP) spectrometer was used to determine all elemental concentrations of phosphorus required in these studies. ASTM Method D 4951 [25] was followed using cobalt at 200 PPM as an internal standard. 

The inductively coupled plasma ion source was developed to accomplish exactly the opposite of the two soft ionization methods just described. Molecules are reduced to their atomic (i.e. elemental) components through the application of intense energy. Masses corresponding to elements of interest (e.g. 30.974 for phosphorus) are then specifically monitored. 

Quantitative organic phosphorus determination by inductively coupled plasma high-resolution mass spectrometry... 

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