REAGENT WATER (1080)/Methods for Preparation of Reagent Water

1080 REAGENT WATER

1080 A. Introduction
One of the most important aspects of analysis is the preparation of reagent water to be used for dilution of reagents and for blank analysis. Reagent water is water with no detectable concentration of the compound or element to be analyzed at the detection level of the analytical method. Reagent water should be free of substances that interfere with analytical methods. The quality of water required is related directly to the analysis being made. Requirements for water quality may differ for organic, inorganic, and biological constituents depending on the use(s) for which the water is intended. Any method of preparation of reagent water is acceptable provided that the requisite quality can be met. Improperly maintained systems may add contaminants. Reverse osmosis, distillation, and deionization in various combinations all can produce reagent water when used in the proper arrangement. Ultraltration and/or ultraviolet treatment also may be used as part of the process. Section 1080 provides general guidelines for the preparation of reagent water. Table 1080:I lists commonly available processes for water purication and major classes of contaminants removed by purication. For details on preparing water for microbiological tests, see Section 9020B.3d.

TABLE 1080:I. WATER PURIFICATION PROCESSES Major Classes of Contaminants* Process Distillation Deionization Reverse osmosis Carbon adsorption Filtration Ultraltration Ultraviolet oxidation Dissolved Ionized Solids GE E G P P P P Dissolved Ionized Gases P E P P P P P Dissolved Organics G P G GE P G# GE** Particulates E P E P E E P Bacteria E P E P E E G Pyrogens/ Endotoxins E P E P P E P

Permission to use this table from C3-A2, Vol. 11, No. 13, Aug. 1991, Preparation and Testing of Reagent Water in the Clinical Laboratory - Second Edition has been granted by the National Committee for Clinical Laboratory Standards. The complete current standard may be obtained from National Committee for Clinical Laboratory Standards, 771 E. Lancaster Ave., Villanova, PA 19085. * E Excellent (capable of complete or near total removal), G Good (capable of removing large percentages), P Poor (little or no removal). Resistivity of water puried by distillation is an order of magnitude less than water produced by deionization, due mainly to the presence of CO2 and sometimes H2S, NH3, and other ionized gases if present in the feedwater. Resistivity of dissolved ionized solids in the product water depends on original feedwater resistivity. Activated carbon removes chlorine by adsorption. When used in combination with other purication processes, special grades of activated carbon and other synthetic adsorbents exhibit excellent capabilities for removing organic contaminants. Their use, however, is targeted toward specic compounds and applications. # Ultralters have demonstrated usefulness in reducing specic feedwater organic contaminants based on the rated molecular weight cut-off of the membrane. ** 185 nm ultraviolet oxidation (batch process systems) is effective in removing trace organic contaminants when used as post-treatment. Feedwater makeup plays a critical role in the performance of these batch processors. 254 nm UV sterilizers, while not physically removing bacteria, may have bactericidal or bacteriostatic capabilities limited by intensity, contact time, and ow rate.

1080 B. Methods for Preparation of Reagent Water

1. Distillation

Prepare laboratory-grade distilled water by distilling water from a still of all-borosilicate glass, fused quartz, tin, or titanium. To remove ammonia distill from an acid solution. Remove CO2 by boiling the water for 15 min and cooling rapidly to room temperature; exclude atmospheric CO2 by
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using a tube containing soda lime or a commercially available CO2-removing agent.* Boiling the water may add other impurities by leaching impurities from the container. Freshly replaced lters, cartridges and resins initially can release impurities. Pretreat feedwater and

* Ascarite II, Fisher Scientic Co., or equivalent.

REAGENT WATER (1080)/Reagent Water Quality

provide periodic maintenance to minimize scale formation within the still. Pretreatment may be required where the feedwater contains signicant concentrations of calcium, magnesium, and bicarbonate ions; it may involve demineralization via reverse osmosis or ion exchange.
2. Reverse Osmosis

Reverse osmosis is a process in which water is forced under pressure through a semipermeable membrane removing a portion of dissolved constituents and suspended impurities. Product water quality depends on feedwater quality. Select the reverse osmosis membrane module appropriate to the characteristics of the feedwater. Obtain rejection data for contaminants in the feedwater at the operating pressure to be used in preparing reagent water. Set overall water production to make the most economical use of water without compromising the nal quality of the permeate. Selection of spiral-wound or hollow ber congurations depends on fouling potential of the feedwater. Regardless of conguration used, pretreatment may be required to minimize membrane fouling with colloids or particulates and to minimize introduction of chlorine, iron, and other oxidizing compounds that may degrade reverse osmosis membranes. Periodic ushing of the membrane modules is necessary.
3. Ion Exchange

position the anion exchanger downstream of the cation exchanger to remove leachates from the cation resin. Proper bed sizing is critical to the performance of the resins. In particular, set the length-to-diameter ratio of the bed in accordance with the maximum process ow rate to ensure that optimal face velocities are not exceeded and that sufcient residence time is provided. In applications where the feedwater has signicant quantities of organic matter, remove organics to minimize potential fouling of the resins. Possible pretreatments include preltration, distillation, reverse osmosis, or adsorption.
4. Adsorption

Prepare deionized water by passing feedwater through a mixedbed ion exchanger, consisting of strong anion and strong cation resins mixed together. When the system does not run continuously, recirculate product water through ion-exchange bed. Use separate anion and cation resin beds in applications where resin regeneration is economically attractive. In such instances,

Adsorption is generally used to remove chlorine and organic impurities. It is accomplished typically with granular activated carbon. Efciency of organics removal depends on the nature of the organic contaminants, the physical characteristics of the activated carbon, and the operating conditions. In general, organics adsorption efciency is inversely proportional to solubility and may be inadequate for the removal of low-molecularweight, polar compounds. Performance differences among activated carbons are attributable to the use of different raw materials and activation procedures. Select the appropriate activated carbon with regard to these differences. Even with optimum activated carbon, proper performance will not be attained unless the column is sized to give required face velocity and residence time at the maximum process ow rate. Use of activated carbon may adversely affect resistivity. This effect may be controlled by use of reverse osmosis, mixed resins, or special adsorbents. To achieve the lowest level of organic contamination, use mixtures of polishing resins with special carbons in conjunction with additional treatment steps, such as reverse osmosis, natural carbons, ultraviolet oxidation, or ultraltration.

1080 C. Reagent Water Quality

1. Quality Guidelines
TABLE 1080:II. REAGENT WATER SPECIFICATIONS Quality Parameter Resistivity, megohm-cm at 25C Conductivity, mho/cm at 25C SiO2, mg/L High 10 0.1 0.05 Medium 1 1 0.1 Low 0.1 10 1

Several guidelines for reagent water quality, based on contaminant levels, are available, but the nal test is the appropriateness for the analysis. Table 1080:II lists some characteristics of various qualities of reagent water. High-quality reagent water, having a minimum resistivity of 10 megohms-cm, 25C (in line), typically is prepared by distillation, deionization, or reverse osmosis treatment of feedwater followed by polishing with a mixed-bed deionizer and passage through a 0.2- m-pore membrane lter. Alternatively treat by reverse osmosis followed by carbon adsorption and deionization. Determine quality at the time of production. Mixed-bed deionizers typically add small amounts of organic matter to water, especially if the beds are fresh. Resistivity should be 10 megohm-cm at 25C, measured in-line. Resistivity measurements will not detect organics or nonionized contaminants, nor will they provide an accurate assessment of ionic contaminants at the microgram-per-liter level. Medium-quality water typically is produced by distillation or deionization. Resistivity should be 1 megohm-cm at 25C.
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Low-quality water should have a minimum resistivity of 0.1 megohm-cm, and may be used for glassware washing, preliminary rinsing of glassware, and as feedwater for production of higher-grade waters. The pH of high- or medium-quality water cannot be measured accurately without contaminating the water. Measure other constituents as required for individual tests. High-quality water cannot be stored without signicant degradation; produce it continuously and use it immediately after processing. Medium-quality water may be stored, but keep

LABORATORY OCCUPATIONAL HEALTH AND SAFETY (1090)/Introduction

storage to a minimum and provide quality consistent with the intended use. Store only in materials that protect the water from contamination, such as TFE and glass for organics analysis or plastics for metals. Store low-quality water in materials that protect the water from contamination.

2. Bibliography
AMERICAN SOCIETY FOR TESTING AND MATERIALS. 1991. Annual Book of ASTM Standards, Vol. 11.01, D 1193-91. American Soc. Testing & Materials, Philadelphia, Pa.

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