Water content analytical procedures

The analytical procedure is checked by analyses of method blanlcs to assure that secondary contamination by the analytes to be determined is avoided or minimized. Because the water content of the CRM matrix to be analyzed may vary from one laboratory to another (dependent on the local humidity and temperature), the water content has to be determined. Accordingly, at least three independent samples are kept at I05°C for 2 h, then allowed to cool to ambient temperature in a desiccator and the water loss is determined. The certified values are generally reported on a dry mass basis. 

Plant material water contents range from high (>90%, e.g. vegetables) to low (< 10%, e.g. straw, herbs, tea, hops, etc.). Thus the ratio between the analytes (residues) and the organic matter potentially interfering with the analysis is very different for, e.g., cucumber and camomile tea. Other ingredients in plant materials such as acids, oil, sugars, starch or substances typically for the taste and effect of plant materials may have properties similar to those of the analytes and thus interfere in or influence the cleanup procedures. 

To reduce the effort, another validation procedure is used for extension of the German multi-residue method to a new analyte. Actually, more than 200 pesticides can be analyzed officially with this method, which is the up-to-date version of the better known method DFG SI9. A typical validation is performed by at least three laboratories, which conduct fortification experiments at the same three levels with at least four representative matrices. These representative matrices are commodities with high water content (e.g., tomato), fruits with high acid content (e.g., lemon), dry crops (e.g., cereals) and commodities with high fat content (e.g., avocado). 

Glacial acetic acid, pure or mixed with other solvents, is one of the most attractive solvents for the titration of amines. Commercial acetic acid containing not more than 1% of water (Karl Fischer titration check) can be used in normal practice for the highest accuracy, however, the water content must be lowered to about 0.01% by addition of acetic anhydride and standing for 24 h not more than the stoichiometric amount of acetic anhydride should be used in order to avoid possible reactions with active hydrogen-containing analyte components such as primary or secondary amines or alcohols. A similar procedure is followed in the preparation of perchloric acid titrant from the commercial... 

There are several potential sources of error in these methods. The filters routinely used have a relatively high and somewhat variable sulfate content, so that, at concentrations lower than 10 Mg/m and sampling periods less than 24 h, the reliability of tlie sulfate measurement is reduc. Several different types of filtering media adsorb sulfur dioxide during the ftrst few hours of sampling this alters the amount of sulfate observed. This interference can become critical when sampling periods are less than 24 h and the concentration ratio of sulfur dioxide to sulfate is greater than 5 1. Interference can also be introduced by hot-water extraction when reduced sulfur compounds like sulfite are present, because they are oxidized to sulfates in this process. Another possible error source is that some of the various analytic procedures us for sulfate determination may be influenced by other substances also present in the particulate matter. 

Water Content — 0.20% by wt. This limit insures that the material is miscible without turbidity with 19 volumes of 99% heptane at 20°. Determination is conducted by Karl Fischer Method, as described in ASTM D1364 and here as Spec MIL-E-463B, Procedure 4.3 7 uoder ETHANOL, Analytical Procedures... 

The aim of validation of an analytical procedure is to demonstrate that the method employed in any product testing, such as the identification, control of impurities, assay, dissolution, particle size, water content, or residual solvents, is validated in the most important characteristics. Identification tests, quantitative tests for impurities content, limit tests for control of impurities, and quantitative tests of the active moiety in samples of pharmaceutical product are the most common types of analytical procedures that validation addresses [1]. 

Water Content. See under Moisture and Moisture, Analytical Procedures in Vol 8, M149-L to M154-L... 

The degree of hydration of the products from these preparations and the water content given by analytical procedures depends upon the heat treatment (method and history) of the product. A sample subjected to TGA (thermal gravimetric analysis) looses water almost continually from room temperature until it becomes the completely anhydrous heteropolytungstate salt at about 400°C. On the other hand, these crystals lose some lattice water rapidly upon removal from the mother liquor and exposure to air even at room temperature. 

The choice of analytical procedure for the determination of metals in water using AAS is dictated by two important factors, (a) The suspended solids and organic content of the water determines whether a pretreatment is necessary, (b) The particular metal and its level of concentration in the sample decides whether a pre-concentration technique is required. In addition, this factor may be useful in choosing between employing a flame or flameless mode of analysis. 

Analytical Procedure Microscopic Examination Place a small amount of a crushed tablet or capsule contents on a slide, mix with a drop of water, and cover carefully with a cover-slip avoiding trapped air bubbles. Observe under low-power magnification. Effervescence will be obvious. If crystalline material is visible, note if it is water-soluble. Check the pH of the solution. An alkaline reaction may indicate the presence of a sodium salt of an acidic drug. Introduce a small drop of silver nitrate solution along one edge of the cover-slip a visible precipitate indicates the possible presence of a hydrochloride salt of a basic drug. 

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