Metals, determination inductively coupled plasma

Another result of the requirements to distribute homogeneous test material is that some pretreatment steps usually performed on routine samples are not done on the interlaboratory sample. For example, in interlaboratory rounds for the determination of metals by inductively coupled plasma, the test material is often a solution of the metals in water. Often a method requires extraction of the metals by acid digestion of the field sample, a procedure that will have significant uncertainty in terms of recovery of analyte. 

Drug A formulation lots were then examined for evidence of iron as well as other transition metal ions. Inductively coupled plasma-mass spectroscopy (ICP-MS) was used initially in a semiquantitative scanning mode. This mode of detection allows for determination of the elements sodium through mercury with detection limits of about Ippb with absolute errors typically about 30%. The three manufactured batches shown in Table 3 were examined. With the exception of iron, no first-, second-or third-row transition metal ion was found in any lot at greater than 2 ppb. Most transition metals were undetectable. Iron, in contrast, was detected at between 10 and 30 ppb. Iron levels were quantitated more accurately by using the method of standard... 

Analyses for metals in meat and meat products are carried out by atomic spectrometry, generally after dry-ashing and solubilization of the ash in acid. Sodium and potassium, being present at relatively high levels in meats, are determined by atomic emission spectrometry, while other metals, such as cadmium, copper, iron, lead, and zinc, are determined by atomic absorption spectrometry. An alternative method applicable to most metals is inductively coupled plasma atomic emission spectrometry. 

Dressier, V. L., Pozebon, D., and Curtins, A. J. (1998). Determination of heavy metals by inductively coupled plasma mass spectrometry after on-line separation and pre- concentration. Spectrochim.Acta, Part B 53(11), 1527. 

Oxygen and nitrogen also are deterrnined 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 deterrnined by the Kjeldahl technique (19). Phosphoms 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). 

Nickel also is deterrnined by a volumetric method employing ethylenediaminetetraacetic acid as a titrant. Inductively coupled plasma (ICP) is preferred to determine very low nickel values (see Trace AND RESIDUE ANALYSIS). The classical gravimetric method employing dimethylglyoxime to precipitate nickel as a red complex is used as a precise analytical technique (122). A colorimetric method employing dimethylglyoxime also is available. The classical method of electro deposition is a commonly employed technique to separate nickel in the presence of other metals, notably copper (qv). It is also used to estabhsh caUbration criteria for the spectrophotometric methods. X-ray diffraction often is used to identify nickel in crystalline form. 

Rubidium metal is commeicially available in essentially two grades, 99 + % and 99.9 + %. The main impurities ate other alkali metals. Rubidium compounds are available in a variety of grades from 99% to 99.99 + %. Manufacturers and suppliers of mbidium metal and mbidium compounds usually supply a complete certificate of analysis upon request. Analyses of metal impurities in mbidium compounds are determined by atomic absorption or inductive coupled plasma spectroscopy (icp). Other metallic impurities, such as sodium and potassium, are determined by atomic absorption or emission spectrograph. For analysis, mbidium metal is converted to a compound such as mbidium chloride. 

A novel interface to connect a ce system with an inductively coupled plasma mass spectrometric (icpms) detector has been developed (88). The interface was built using a direct injection nebulizer (din) system. The ce/din/icpms system was evaluated using samples containing selected alkah, alkaline earths, and heavy-metal ions, as well as selenium (Se(IV) and Se(VI)), and various inorganic and organic arsenic species. The preliminary results show that the system can be used to determine metal species at ppt to ppb level. 

The Production Department was not amused, because lower values had been expected. Quality Control was blamed for using an insensitive, unse-lective, and imprecise test, and thereby unnecessarily frightening top management. This outcome had been anticipated, and a better method, namely polarography, was already being set up. The same samples were run, this time in duplicate, with much the same results. A relative confidence interval of 25% was assumed. Because of increased specificity, there were now less doubts as to the amounts of this particular heavy metal that were actually present. To rule out artifacts, the four samples were sent to outside laboratories to do repeat tests with different methods X-ray fluorescence (XRFi °) and inductively coupled plasma spectrometry (ICP). The confidence limits were determined to be 10% resp. 3%. Figure 4.23 summarizes the results. Because each method has its own specificity pattern, and is subject to intrinsic artifacts, a direct statistical comparison cannot be performed without first correcting the apparent concentrations in order to obtain presumably true... 

Caroli S, Forte G, Iamiceu AL, Galoppi B 1999) Determination of essential and potentially toxic trace elements in honey by inductively coupled plasma-based techniques. Talanta 50 327-336. Chiswell B, Johnson D (1994) Manganese. In Seiler HG, Sigel A, Sigel H, eds. Handbook on metals in clinical and analytical chemistry. Dekker, New York. 

Measurement techniques that can be employed for the determination of trace metals include atomic absorption spectrometry, anodic stripping voltammetry, differential pulse cathodic stripping voltammetry, inductively coupled plasma atomic emission spectrometry, liquid chromatography of the metal chelates with ultraviolet-visible absorption and, more recently, inductively coupled plasma mass spectrometry. 

Many of the published methods for the determination of metals in seawater are concerned with the determination of a single element. Single-element methods are discussed firstly in Sects. 5.2-5.73. However, much of the published work is concerned not only with the determination of a single element but with the determination of groups of elements (Sect. 5.74). This is particularly so in the case of techniques such as graphite furnace atomic absorption spectrometry, Zeeman background-corrected atomic absorption spectrometry, and inductively coupled plasma spectrometry. This also applies to other techniques, such as voltammetry, polarography, neutron activation analysis, X-ray fluroescence spectroscopy, and isotope dilution techniques. 

Unlike halogenated solvents, it does not produce noxious substances in the inductively coupled plasma, has a very low aqueous solubility, and yields hundredfold concentration in one step. Detection limits ranged from 0.02 jtg/l (cadmium) to 0.6 pg/1 (lead). The results indicate that the proposed procedure should be useful for the precise determination of metals in oceanic water, although a higher sensitivity would be necessary for lead and cadmium. 

Mykytiuk et al. [184] have described a stable isotope dilution sparksource mass spectrometric method for the determination of cadmium, zinc, copper, nickel, lead, uranium, and iron in seawater, and have compared results with those obtained by graphite furnace atomic absorption spectrometry and inductively coupled plasma emission spectrometry. These workers found that to achieve the required sensitivity it was necessary to preconcentrate elements in the seawater using Chelex 100 [121] followed by evaporation of the desorbed metal concentrate onto a graphite or silver electrode for isotope dilution mass spectrometry. 

Brief mention has been made, particularly in connection with the inductively coupled plasma atomic absorption spectrometric technique, of the need to preconcentrate seawater samples prior to the determination of metals, in order to achieve adequate detection limits. 

Table 21 reports the ash content and ash composition (determined by inductively coupled plasma-atomic emission spectroscopy, ICP-AES) for all of the calcined cokes used to fabricate the test graphites. It can be seen that the amount of ash and its make-up are variable, but are within the range observed for petroleum-based calcined cokes. Although the ash contents in all of the calcined cokes appear rather high, these materials may still be acceptable because many of the metallic species are driven off during graphitization. This aspect is addressed in the next section. 

List the advantages and disadvantages of dc-arc spectrometry and inductively coupled plasma spectrometry, when used to determine trace metals in solid samples. Indicate the main reasons for preferring ICP spectrometry, in most cases. 

A Thermo Finnigan Element 2 Inductively Coupled Plasma Sector-Field Mass Spectrometer (ICP-SF-MS) with guard electrode was employed for trace element analyses. RSD values derived from internal check standard never exceeded 10%. Accuracy was better than 15% for all elements as determined by analyzing the certified reference standard NWRI TM-RAIN 95 trace metal fortified rainwater, every 5 to 8 samples. 

The content of heavy metals in sediments was determined by sample digestion with 10 ml of the mixture of HCI04, HCI, HN03 and HF at 200°C, followed by Inductively Coupled Plasma Emission Spectrometry (ICP) (ACME, 2003). 

Goossens J, Moens L, Dams R. Inductively coupled plasma mass spectrometric determination of heavy metals in soil and sludge candidate reference materials. Anal. Chim. Acta 1995 304 307-315. 

Once the sample is in solution in the acid and the digest made up to a standard volume the determination of metals is completed by standard procedures such as atomic absorption spectrometry or inductively coupled plasma optical emission spectrometry. 

The major anions and cations in seawater have a significant influence on most analytical protocols used to determine trace metals at low concentrations, so production of reference materials in seawater is absolutely essential. The major ions interfere strongly with metal analysis using graphite furnace atomic absorption spectroscopy (GFAAS) and inductively coupled plasma mass spectroscopy (ICP-MS) and must be eliminated. Consequently, preconcentration techniques used to lower detection limits must also exclude these elements. Techniques based on solvent extraction of hydrophobic chelates and column preconcentration using Chelex 100 achieve these objectives and have been widely used with GFAAS. 

Several methods have been used to determine the number and position of metal atoms affixed to the protein surface. The number of metal atoms is commonly determined by atomic absorption analysis [16] or by inductively coupled plasma (ICP) atomic emission analysis [15]. Under favorable circumstances, the metal ratios in modified derivatives can be determined by UV-vis... 

Jackson SE, Gunther D (2003) The nature and sources of laser induced isotopic fractionation in laser ablation-multicollector-inductively coupled plasma-mass spectrometry. J Anal At Spectrom 18 205-212 Jiang S-J, Houk RS, Stevens MA (1988) Alleviation of overlap interferences for determination of potassium isotope ratios by Inductively-Coupled Plasma Mass Spectrometry. Anal Chem 60 1217-1220 Lam JWH, Horlick G (1990) A comparison of argon and mixed gas plasmas for inductively coupled plasma-mass spectrometry. Spectrochim Acta Part B 45 1313-1325 Langmuir I, Kingdon KH(1925) Thermionic effects caused by vapours of alkali metals. Phil Trans R Soc A107 61-79... 

Determination of Metals and Trace Elements in Water and Wastes by Inductively Coupled Plasma-Atomic... 

A binder—free Na-Y zeolite with Si/Al ratio of 2.29 was obtained from Strem Chemical Co., La,Na—Y and Cs,Na-Y zeolites were prepared by exchanging Na-Y zeolite with LaCls and CsCl solution at room temperature. The percentage of metal ion exchanged in a zeolite has been determinated by Inductively-Coupled-Plasma Atomic Emission Spectroscopy and the number is used as prefix for the samples, e.g., Cs exchanged level of 667. is represented as 66Cs,Na-Y sample. 

Martin TD, Brockhoff CA, Creed JT, et al. 1992. Determination of metals and trace elements in water and wastes by inductively coupled plasma-atomic emission spectrometry. In Smoley KC, ed. Methods for the determination of metals in environmental samples. Boca Raton, FL CRC Press, 33-78. 

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