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1080 REAGENT WATER*

1080 A. Introduction

One of the most important aspects of analysis is preparing the Use any method to prepare reagent water that can meet the
reagent water used to prepare and dilute reagents and prepare applicable quality requirements. Various combinations of re-
blanks. Reagent water is water with no detectable concentration verse osmosis, distillation, and deionization can produce re-
of the compound or element to be analyzed (i.e., it is below the agent water, as can ultrafiltration and/or ultraviolet irradia-
analytical methods detection level). Reagent water should also tion. Keep in mind, however, that improperly operated or
be free of substances that interfere with analytical methods. maintained water purification systems may add rather than
However, its overall quality (concentrations of organic, inor- remove contaminants.
ganic, and biological constituents) will depend on the waters This section provides general guidelines for preparing reagent
intended use(s). water. Table 1080:I lists commonly available water purification
processes and the major classes of contaminants that they re-
move. For details on preparing water for microbiological tests,
* Reviewed by Standard Methods Committee, 2011. see Section 9020B.4d.

1080 B. Methods for Preparing Reagent-Grade Water

1. Distillation acid solution. Remove CO2 by boiling the water for 15 min
and cooling rapidly to room temperature; exclude atmospheric
Distillation is the process of heating a liquid until it boils, CO2 by using a tube containing soda lime or a commercially
capturing and cooling the resultant hot vapors, and collecting the available CO2-removing agent.*
condensed vapors. Laboratory-grade distilled water should be
generated in a still made of all-borosilicate glass, fused
quartz, tin, or titanium. To remove ammonia, distill from an * Ascarite II, Fisher Scientific Co., or equivalent.

TABLE 1080:I. WATER PURIFICATION PROCESSES


Major Classes of Contaminants*
Dissolved Dissolved Dissolved Pyrogens/
Process Ionized Salts Ionized Gases Organics Particulates Bacteria Endotoxins
Distillation GE P G E E E
Deionization E E P P P P
Reverse osmosis G P G E E E
Carbon adsorption P P GE P P P
Filtration P P P E E P
Ultrafiltration P P G# E E E
Ultraviolet oxidation P P GE** P G 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, Lancaster Ave.,771 E. 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).
The resistivity of water purified via distillation is an order of magnitude less than that in water produced via deionization, mainly due to the presence of CO2 and sometimes
H2S, NH3, and other ionized gases (if present in feedwater).
The resistivity of dissolved ionized solids in product water depends on original feedwater resistivity.
Activated carbon removes chlorine via adsorption.
When used with other purification processes, special grades of activated carbon and other synthetic adsorbents are excellent at removing organic contaminants. Their use,
however, is targeted toward specific compounds and applications.
# Ultrafilters reduce specific feedwater organic contaminants based on the membranes rated molecular weight cut-off.
** 185-nm UV oxidation (batch process) removes trace organic contaminants effectively when used as post-treatment. Feedwater makeup plays a critical role in their
performance.
While 254-nm UV sterilizers do not physically remove bacteria, they may have bactericidal or bacteriostatic capabilities limited by intensity, contact time, and flow rate.

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Impurities may be added to the water during boiling if they bed sizing is critical to resin performance. Be sure the beds
leach from the container. Also, freshly replaced filters, car- length-to-diameter ratio is in accordance with the maximum
tridges, and resins initially can release impurities. Pretreat feed- process flow rate to ensure that optimal face velocities are not
water and maintain still periodically to minimize scale forma- exceeded and that residence time is sufficient.
tion. Pretreatment may be required if the feedwater contains If the system does not generate reagent water continuously,
significant concentrations of calcium, magnesium, and bicarbon- recirculate the water through the ion exchanger. If resin regen-
ate ions; it may involve demineralization via reverse osmosis or eration is economically attractive, use separate anion and cation
ion exchange. resin beds, and position the anion exchanger downstream of the
cation exchanger to remove leachates from the cation resin. If the
2. Reverse Osmosis feedwater contains significant quantities of organic matter, re-
move the organics first to minimize the potential for resin foul-
In reverse osmosis, water is forced under pressure through a ing. Organics can be removed via prefiltration, distillation, re-
semipermeable membrane, thereby removing some dissolved verse osmosis, or adsorption. If using commercially prepared
constituents and suspended impurities. The reagent water quality resin columns, follow suppliers recommendations for monitor-
will depend on both feedwater quality and the type and condition ing QC of reagent water from specific equipment.
of membranes used.
Reverse osmosis membranes are available in both spiral- 4. Adsorption
wound and hollow-fiber configurations; the choice depends on
the feedwaters characteristics and fouling potential. Obtain re- In adsorption, water is fed into a reactor filled with an
jection data for feedwater contaminants (levels of salt and im- adsorbent material (typically, granular activated carbon, al-
purities that will pass through the membranes compared to though some resins and other manmade adsorbents are used in
feedwater levels) at the operating pressure that will be used to specific applications). Chlorine and other organic impurities
prepare reagent water. Set the water-production rate to make the are drawn from the water to the surface of the adsorbent. How
most economical use of feedwater without compromising per- well the process works depends on the organic contaminants
meate (reagent water) quality. involved, the activated carbons physical characteristics, and
Pretreatment steps (e.g., filtration) may be needed to minimize the operating conditions. In general, organics-adsorption ef-
membrane fouling (due to colloids or particulates) and/or deg- ficiency is inversely proportional to the solubility of the
radation (due to chlorine, iron, and other oxidizing compounds). organics in water and the adsorption process may be inade-
Also, the membrane modules need to be backwashed periodi- quate for removing low-molecular-weight, polar compounds.
cally to clean the surface of the membranes. If using a commer- Performance differences among activated carbons are attrib-
cially available reverse osmosis system, follow manufacturers utable to the raw materials and activation procedures. Even
instructions for quality control (QC) and maintenance. with an optimal activated carbon, proper performance will not
be attained unless the column is sized to provide required face
3. Ion Exchange velocity and residence time at the maximum process flow rate.
If using commercial sorbent systems, follow suppliers rec-
In an ion exchange process, water passes through a reactor ommended flow and QC steps.
containing negatively charged (anionic) and/or positively Using activated carbon may adversely affect the reagent wa-
charged (cationic) resins. Targeted ions in the water are substi- ters resistivity. This effect may be controlled via reverse osmo-
tuted with specific ions on the resins (ones acceptable in treated sis, mixed resins, or special adsorbents. To minimize organic
water systems), thereby purifying the water. To prepare deion- contamination, use mixtures of polishing resins with special
ized water, direct feedwater through a mixed-bed ion exchanger, carbons and additional treatment steps (e.g., reverse osmosis,
which contains both strong anion and strong cation resins. Proper natural carbons, ultraviolet oxidation, or ultrafiltration).

1080 C. Reagent Water Quality

1. Quality Guidelines deionization, or reverse osmosis of feedwater followed by


mixed-bed deionization and membrane filtration (0.2-m pore).
Guidelines for reagent water vary with the intended use.1
Table 1080:II lists some characteristics of various qualities of
reagent water. In general, low-quality reagent water has a min- TABLE 1080:II. REAGENT WATER SPECIFICATIONS
imum resistivity of 0.1 megohm-cm at 25C. It may be used to
Quality Parameter High Medium Low
wash glassware, rinse glassware (as a preliminary step), and as a
source to produce higher-grade waters. Resistivity, megohm-cm 10 1 0.1
Medium-quality reagent water typically is produced via distilla- at 25C
tion or deionization. Resistivity should be 1 megohm-cm at 25C. Conductivity, mho/cm 0.1 1 10
High-quality reagent water has a minimum resistivity of 10 at 25C
SiO2, mg/L 0.05 0.1 1
megohms-cm at 25C. It typically is prepared via distillation,

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It also could be prepared via reverse osmosis followed by carbon High-quality water cannot be stored without degrading signif-
adsorption and deionization. icantly. Medium-quality water may be stored, but keep storage
Mixed-bed deionizers typically add small amounts of organic time to a minimum and make sure quality remains consistent
matter to water, especially if the beds are fresh, so determine with the intended use. Only store it in materials that protect the
reagent water quality immediately after preparation. Its resistiv- water from contamination (e.g., TFE and glass for organics
ity (measured in-line) should be 10 megohm-cm at 25C. analysis or plastics for metals).
However, resistivity measurements do not detect organics or
nonionized contaminants, nor accurately assess ionic contam- 2. Reference
inants at the microgram-per-liter level.
The pH of high- or medium-quality water cannot be measured 1. AMERICAN SOCIETY FOR TESTING AND MATERIALS. 2006. Annual Book
accurately without contaminating the water, so measure other of ASTM Standards, Vol 11.01, D 1193-06. American Soc. Testing
constituents required for individual tests. & Materials, W. Conshohocken, Pa.

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