ICPAE

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The use of y-ray induced radical pol5unerization proved to be a successful alternative for the radical co-polymer-ization of metal complexes with ligands containing acrylic C—C double bonds [100-102,129,130]. In particular, the palladium(II) complex cw-[PdCl2(ICPA)2] (1, Scheme 4) was co-polymerized in DMF solution with DMA and MBAA (cross-linker, 4% mol), with no degradation of the metal center [100,101]. 

Multi-Element Analytical Scheme The 76 elements analyzed include 39 elements originally analyzed in the RGNR Projects, and 37 new elements. The analytical scheme is based largely on ICPMS, ICPAES and XRF, supplemented with other techniques (Table 1). The lower levels of detection of all elements are less than their crustal abundances (Table 2). 

An additional disadvantage is that unlike ICPAES, only one element at a time can be determined. Suitable instrumentation is listed in Table 1.3. 

Boron has a very simple ICPAES spectrum with the sensitive doublet at 249.7 and 249.8nm being the only useful analytical lines. Between 0.4 and 0.7mg L 1 boron was found in soil extracts. 

Direct ICPAES ICPAES with flow-injection/ 11.7 2 8.6 1.6 65 18... 

TABLE 14.2. Electrocatalytic activities of several different catalysts catalysts for MOR in terms of peak potential (iCpa) and peak current (ipa) (from Ref. 33). 

In the inductively coupled plasma atomic emission spectroscopy (ICPAES) method (ASTM DD 5600), a sample of petroleum coke is ashed at 700°C (1292°F) and the ash is fused with lithium borate. The melt is dissolved in dilute hydrochloric acid, and the resulting solution is analyzed by inductively coupled plasma atomic emission spectroscopy using aqueous calibration standards. Because of the need to fuse the ash with lithium borate or other suitable salt, the fusibility of ash may need attention (ASTM D1857). 

Li or a Li compound in the flame gives a bright crimson color due to its emission of670.8 nm photons produced by the short-lived species LiOH. This is the property that allows for the spectrophotometric determination of Li by atomic absorption spectroscopy (AAS) down to 20 ppb. Inductively-coupled plasma emission spectroscopy (ICPAES), inductively-coupled plasma mass spectroscopy (ICPMS), and ion chromatography (IC) improve this limit to about 0.1 ppb. A spot test for detection of Li down to 2 ppm is provided by basic KIO4 plus FeCl3. 

Analysis. Na or a Na compound in the flame gives a bright yellow color due to its emission of 589.0 and 589.6 nm photons. This is the property that allows for the spectrophotometric determination of Na by emission or absorption flame or plasma spectroscopy. AAS and ETAAS are capable down to 10 ppb. ICPAES extends this to 1 ppb, and a limit of detection of 0.1 ppb can be obtained by ICPMS and IC. A spot test for 250 ppm or more can... 

Analysis. K or a K compound in the flame gives a reddish-violet (lilac) color. This is due to its emission of404.4,404.7, 766.5, and 769.9 nm photons. These photon lines allow for the determination of K by AA (limit of detection = 20 ppb), ETAAS (1 ppb), and ICPAES (0.1 ppb). This latter limit is also attainable by ICPMS and IC. Spots tests with sodium hexanitritocobaltate(III) and dipicrylamine both detect 100 ppm of K. 

Analysis. Colorimetric methods provide for the determination of Al down to 10 ppb. AAS will analyze for Al down to 50 ppb, ETAAS to 10 ppb, and ICPAES to 1 ppb. ICPMS improves upon this by going down to 0.1 ppb. Alizarin is a reagent which provides for a spot test of Al dovm to 20 ppm. Al+ can also be detected in a spot test by morin in methanol down to 10 ppm. 

Analysis. Colorimetric analysis of Ga permits detection of 20 ppb. Ga or a Ga compound in the flame gives a violet (lilac) color. This is due to its emission of 414.0 nm photons. This photon line allows for the spectrophotometric determination of Ga by AAS, which is sensitive to about 10 ppm. ETAAS increases this sensitivity to 5 ppb, and ICPAES to about 1 ppb, with ICPMS going as low as 0.1 ppb. Rhodamine B is a reagent which facilitates the spottest detection at a level of 10 ppm or above. 

Analysis. The colorimetric method for In is capable of a detection limit of 20 ppb. Indium or an In compound in the flame gives an indigo blue color (451.1 nm). This photon line allows for the spectrophotometric determination ofinby AAS (atomic absorption flame spectroscopy). The method is sensitive to about 300 ppb. With ETAAS, this limit drops to 10 ppb, as it does with ICPAES. ICPMS drops the limit to 0.01 ppb. Alizarin detects In, as well as Al, but the reaction with Al can be masked by addition of F to a spot test. The limit of detection is about 1 ppm. 

Analysis. Atomic absorption, emission, and mass spectrographic separation are the most sensitive methods for the analysis of Si. Electrothermal atomization-atomic absorption spectroscopy ETAAS has a sensitivity of 10 ppb, ICPAES 1 ppb, and ICPMS 10 ppb. Colorimetric agents permit spectrometric analysis down to about 10 ppb. 

Analysis. The most sensitive techniques for the analysis of Ge include ICPAES (1 ppb) and IGPMS (0.1 ppb). Colorimetric agents (phenylfluo-ronone) and molecular absorption spectroscopy can detect 100 ppb. One of the better spot tests involves treatment of a slightly basic germanate solution with phenolphthalein to produce a red color, then the addition of mannitol which turns the solution colorless. Sensitivity is 100 ppm. A major interference is B. 

Analysis. Colorimetric analysis of Pb with dithizone can be performed down to 200 ppb, with ETAAS and ICPAES going down to 1 ppb, and ICPMS to 0.1 ppb. Spot testing to a detection limit of almost 1 ppm can be carried out using dithizone and KCN. 

Analysis. Colorimetric analysis using rhodamine B for color development permits the determination of Sb down to 50 ppb. ETAAS and ICPAES are capable of a sensitivity of 5 ppb, and ICPMS extends this to 0.1 ppb. 

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