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Laboratories use many different container materials for handling samples during sample preparation. Some materials are more advantageous to use than others. In this part, we'll look at the properties of borosilicate glass, porcelain, quartz, platinum, graphite, and plastics.
Borosilicate glass is used extensively. It is resistant to most acids, but should not be used with HF or boiling H3PO4. As a general rule alkaline solutions should not be heated or stored in borosilicate glass. Borosilicate glass can contribute a variety of contaminants. It should not be heated over temperatures achievable using a hot plate (500 °C). For example, if you need to ash a sample using a muffle furnace, do not use borosilicate glass.
Porcelain is a popular material used for ashing purposes. Porcelain contains Na, K, Al, and Si in increasing concentration. It is typically coated with a glaze which is about 70 % SiO2, with roughly equal amounts of the oxides of Al and Ca, and lesser amounts of Na and K. Attack will occur if the sample contains even minor amounts of the alkali metals. This is made evident by a dulling in the normally shiny surface. If alkalis are present, then the sample is typically treated with conc. H2SO4 prior to ashing. The following should not be heated in porcelain: HF; boiling H3PO4; and the oxides, hydroxides, or carbonates of the alkali or alkaline earth elements. The major advantage or porcelain over glass is that it can be heated up to 1100 °C.
There are two types of quartz -- opaque and transparent.
Use the synthetic type III quartz whenever possible. More details as to the contamination issues around the use of quartz will be discussed in later chapters.
Quartz is typically 99.8+% SiO2. It is attacked by HF, boiling H3PO4, and the alkali and alkaline earth oxides, hydroxides, and carbonates. It can be heated to 1100 °C . Its main advantage over that of porcelain is that major contamination occurs from only Si -- however, this contamination can be significant.
Platinum, although expensive, is a popular container material. It heats up and cools down rapidly, making it excellent for % ash determinations where the % ash is at low levels.
It is resistant to attack by most acids and reagents. Avoid concentrated H3PO4 at high temperatures, HCl + HNO3 mixtures and fusions using Li2CO3, Na2O2, or the alkali hydroxides. Fusions using Na2CO3 are common in addition to fusions using the alkali borates, fluorides, nitrates, and bisulphates. Avoid heating at prolonged temperatures in excess of 1100 °C (m.p. = 1772 °C).
Platinum can be destroyed by heating with metals with which it can alloy. Avoid high temperature heating with samples containing significant levels of any metal that may be in or reduced to the metallic state during the heating process. For example, a sample containing high levels of Cu0 or Cu+2 should be avoided, especially if present in an organic matrix. A sample containing trace levels of Cu in an organic matrix will not ruin the platinum, but it is likely to be lost to the platinum during the ashing process. Since platinum has this alloying tendency, it is best to avoid its use with samples containing elements other than those that have no tendency to form the metal (i.e. - alkali, alkaline and rare earth elements). Platinum is known to contain trace amounts of the other precious metals and should not be used for their preparation. Avoid samples containing Hg any an form. Hg metal is easily formed and alloys very readily at room temperature with platinum. Also avoid ashing samples containing P in any form, including the phosphates.
Graphite is very inexpensive and relatively clean, but very messy to work with. It is an inexpensive way to perform Li2CO3 fusions where the crucible slowly oxidizes away over the course of 7-10 fusions. It is popular because it does not wet by some melts which can be poured out quantitatively. Losses due to the porosity of graphite should exclude its use for ashing samples containing trace metals. Graphite's main advantage to the trace analyst is being a material that can withstand fusions that might destroy platinum. Our chemists use graphite for performing Li2CO3 fusions in the preparation of large numbers of limestone samples for major minor and trace elemental analysis.
Plastics are very important to the trace analyst. Whenever possible, the analyst should attempt to use plastics for sample collection, storage, preparation, and measurement. Their major disadvantage is the inability to be used for high temperature operations, such as ashing or fusion. Table 5.1 shows a summary of the physical properties of some common plastics.
The most popular plastics are PFA and HDPE / LDPE.
PFA has excellent properties, allowing for use in acid digestions up to 250 °C. Typically, PFA is used for acid digestions using either HF, HNO3 or HCl, alone or in combination. The use of higher boiling acids such as H2SO4 and H3PO4 have been reported in PFA, but great care must be taken not to exceed the 250 °C maximum operating temperature. PFA is commonly used in the construction of microwave digestion vessels. Microwave digestions using the higher boiling acids should not be attempted. Digestions using HCLO4 should never be performed in plastics of any kind.
LDPE or HDPE bottles are typically used for containment of the sample digestate after dilution with water. These bottles can withstand solutions of HNO3 that are 10% v/v and lower over extended periods of time (i.e. - years). The caps used for the LDPE and HDPE bottles are made of PP, which is more rigid than the polyethylene and well-suited for its purpose. Unfortunately, the PP cap is not as clean as the PE bottle.
All of the above plastics were part of a study conducted at our laboratories concerning their purity and cleaning properties, further described below.
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