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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
blanks. Reagent water is water with no detectable concentration reverse osmosis, distillation, and deionization can produce
of the compound or element to be analyzed (i.e., it is below the reagent water, as can ultrafiltration and/or ultraviolet irradia-
analytical method’s 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 water’s 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. T1

1080 B. Methods for Preparing Reagent-Grade Water

1. Distillation purities that will pass through the membranes compared to


feedwater levels) at the operating pressure that will be used to
Distillation is the process of heating a liquid until it boils, prepare reagent water. Set the water-production rate to make the
capturing and cooling the resultant hot vapors, and collecting the most economical use of feedwater without compromising per-
condensed vapors. Laboratory-grade distilled water should be meate (reagent water) quality.
generated in a still made of all-borosilicate glass, fused quartz, Pretreatment steps (e.g., filtration) may be needed to minimize
tin, or titanium. To remove ammonia, distill from an acid solu- membrane fouling (due to colloids or particulates) and/or deg-
tion. Remove CO2 by boiling the water for 15 min and cooling radation (due to chlorine, iron, and other oxidizing compounds).
rapidly to room temperature; exclude atmospheric CO2 by using Also, the membrane modules need to be backwashed periodi-
a tube containing soda lime or a commercially available cally to clean the surface of the membranes. If using a commer-
CO2-removing agent.* cially available reverse osmosis system, follow manufacturer’s
Impurities may be added to the water during boiling if they instructions for quality control (QC) and maintenance.
leach from the container. Also, freshly replaced filters,
cartridges, and resins initially can release impurities. Pretreat 3. Ion Exchange
feedwater and maintain still periodically to minimize scale for-
mation. Pretreatment may be required if the feedwater contains
In an ion exchange process, water passes through a reactor
significant concentrations of calcium, magnesium, and bicarbon-
containing negatively charged (anionic) and/or positively
ate ions; it may involve demineralization via reverse osmosis or
charged (cationic) resins. Targeted ions in the water are substi-
ion exchange.
tuted with specific ions on the resins (ones acceptable in treated
water systems), thereby purifying the water. To prepare deion-
2. Reverse Osmosis ized water, direct feedwater through a mixed-bed ion exchanger,
which contains both strong anion and strong cation resins. Proper
In reverse osmosis, water is forced under pressure through a bed sizing is critical to resin performance. Be sure the bed’s
semipermeable membrane, thereby removing some dissolved length-to-diameter ratio is in accordance with the maximum
constituents and suspended impurities. The reagent water quality process flow rate to ensure that optimal face velocities are not
will depend on both feedwater quality and the type and condition exceeded and that residence time is sufficient.
of membranes used. If the system does not generate reagent water continuously,
Reverse osmosis membranes are available in both spiral- recirculate the water through the ion exchanger. If resin regen-
wound and hollow-fiber configurations; the choice depends on eration is economically attractive, use separate anion and cation
the feedwater’s characteristics and fouling potential. Obtain re- resin beds, and position the anion exchanger downstream of the
jection data for feedwater contaminants (levels of salt and im- cation exchanger to remove leachates from the cation resin. If the
feedwater contains significant quantities of organic matter,
remove the organics first to minimize the potential for resin
* Ascarite II, Fisher Scientific Co., or equivalent. fouling. Organics can be removed via prefiltration, distillation,

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REAGENT WATER (1080)/Reagent Water Quality

TABLE 1080:I. WATER PURIFICATION PROCESSES


Major Classes of Contaminants*
Dissolved Dissolved Dissolved Pyrogens/
Process Ionized Salts Ionized Gases Organics Particulates Bacteria Endotoxins

Distillation G–E† P G E E E
Deionization E E P P P P
Reverse osmosis G‡ P G E E E
Carbon adsorption P P§ G–E㛳 P P P
Filtration P P P E E P
Ultrafiltration P P G# E E E
Ultraviolet oxidation P P G–E** 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. 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).
† 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.
㛳 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 membrane’s 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.

reverse osmosis, or adsorption. If using commercially prepared organics in water and the adsorption process may be inade-
resin columns, follow supplier’s recommendations for monitor- quate for removing low-molecular-weight, polar compounds.
ing QC of reagent water from specific equipment. Performance differences among activated carbons are attrib-
utable to the raw materials and activation procedures. Even
4. Adsorption with an optimal activated carbon, proper performance will not
be attained unless the column is sized to provide required face
In adsorption, water is fed into a reactor filled with an velocity and residence time at the maximum process flow rate.
adsorbent material (typically, granular activated carbon, al- If using commercial sorbent systems, follow supplier’s rec-
though some resins and other manmade adsorbents are used in ommended flow and QC steps.
specific applications). Chlorine and other organic impurities Using activated carbon may adversely affect the reagent wa-
are drawn from the water to the surface of the adsorbent. How ter’s resistivity. This effect may be controlled via reverse osmo-
well the process works depends on the organic contaminants sis, mixed resins, or special adsorbents. To minimize organic
involved, the activated carbon’s physical characteristics, and contamination, use mixtures of polishing resins with special
the operating conditions. In general, organics-adsorption ef- carbons and additional treatment steps (e.g., reverse osmosis,
ficiency is inversely proportional to the solubility of the natural carbons, ultraviolet oxidation, or ultrafiltration).

1080 C. Reagent Water Quality

1. Quality Guidelines High-quality reagent water has a minimum resistivity of


10 megohms-cm at 25°C. It typically is prepared via distillation,
Guidelines for reagent water vary with the intended use.1 deionization, or reverse osmosis of feedwater followed by
Table 1080:II lists some characteristics of various qualities of mixed-bed deionization and membrane filtration (0.2-␮m pore).
reagent water. In general, low-quality reagent water has a min- It also could be prepared via reverse osmosis followed by carbon
imum resistivity of 0.1 megohm-cm at 25°C. It may be used to adsorption and deionization.
wash glassware, rinse glassware (as a preliminary step), and as a Mixed-bed deionizers typically add small amounts of organic
source to produce higher-grade waters. matter to water, especially if the beds are fresh, so determine
Medium-quality reagent water typically is produced via dis- reagent water quality immediately after preparation. Its resistiv-
tillation or deionization. Resistivity should be ⬎1 megohm-cm at ity (measured in-line) should be ⬎10 megohm-cm at 25°C.
25°C. However, resistivity measurements do not detect organics or

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REAGENT WATER (1080)/Reagent Water Quality

TABLE 1080:II. REAGENT WATER SPECIFICATIONS High-quality water cannot be stored without degrading signif-
Quality Parameter High Medium Low
icantly. Medium-quality water may be stored, but keep storage
time to a minimum and make sure quality remains consistent
Resistivity, megohm-cm ⬎10 ⬎1 ⬎0.1 with the intended use. Only store it in materials that protect the
at 25°C water from contamination (e.g., TFE and glass for organics
Conductivity, ␮mho/cm ⬍0.1 ⬍1 ⬍10
analysis or plastics for metals).
at 25°C
SiO2, mg/L ⬍0.05 ⬍0.1 ⬍1

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
accurately without contaminating the water, so measure other 1. AMERICAN SOCIETY FOR TESTING & MATERIALS. 2006. Annual Book of
constituents required for individual tests. ASTM Standards; Vol 11.01, D 1193-06. W. Conshohocken, Pa.

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