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SMWW 1080
SMWW 1080
Reagent Water
1080 A. Introduction
One of the most important aspects of analysis is preparing osmosis, distillation, deionization, or ultrafiltration and ultravi-
the reagent water used for blanks and reagents. Reagent water olet irradiation can produce reagent water. Keep in mind, how-
is water with no detectable concentration of the compound or ever, that improperly operated or maintained water purification
element to be analyzed (i.e., it is below the analytical method’s systems may add rather than remove contaminants.
detection level). Reagent water should also be free of substances This section provides general guidelines for preparing reagent
that interfere with analytical methods. However, its overall qual- water. Table 1080:1 lists commonly available water purifica-
ity (concentrations of organic, inorganic, and biological constitu- tion processes and the major classes of contaminants that they
ents) depends on the water’s intended uses. remove. For details on preparing water for microbiological tests,
Use any method to prepare reagent water that meets the appli- see Section 9020 B.4d.
cable quality requirements. Various combinations of reverse
1. Distillation operating pressure that will be used to prepare reagent water. Set
the water-production rate to make the most economical use of feed-
Distillation is the process of heating a liquid until it boils, cap- water without compromising permeate (reagent water) quality.
turing and cooling the resultant hot vapors, and collecting the Pretreatment steps (e.g., filtration) may be needed to minimize
condensed vapors. Laboratory-grade distilled water should be membrane fouling (due to colloids or particulates) and degra-
generated in a still made of all-borosilicate glass, fused quartz, dation (due to chlorine, iron, and other oxidizing compounds).
tin, or titanium. To remove ammonia, distill from an acid solu- Also, the membrane modules need to be backwashed periodically
tion. Remove CO2 by boiling the water for 15 min and cooling to clean the surface of the membranes. If using a commercially
rapidly to room temperature; exclude atmospheric CO2 by using available reverse osmosis system, follow the manufacturer’s
a tube containing soda lime or a commercially available CO2- instructions for quality control (QC) and maintenance.
removing agent (e.g., Ascarite II).
Impurities may leach into water from its container during boil- 3. Ion Exchange
ing. Also, freshly replaced filters, cartridges, and resins initially
can release impurities. Pretreat feedwater and maintain a still In an ion exchange process, water passes through a reactor con-
periodically to minimize scale formation. A demineralization pre- taining negatively charged (anionic), positively charged (cationic)
treatment using reverse osmosis or ion exchange may be required resins, or both. Targeted ions in the water are substituted with spe-
if the feedwater contains significant concentrations of calcium, cific ions on the resins (ones acceptable in treated water systems),
magnesium, and bicarbonate ions. thereby purifying the water. To prepare deionized water, direct
feedwater through a mixed-bed ion exchanger, which contains
2. Reverse Osmosis both strong anion and strong cation resins. Proper bed sizing is
critical to resin performance. Be sure the bed’s length-to-diameter
During reverse osmosis, water is forced under pressure through ratio is in accordance with the maximum process flow rate to
a semipermeable membrane, thereby removing some dissolved ensure that optimal face velocities are not exceeded and that
constituents and suspended impurities. The resultant reagent residence time is sufficient.
water quality depends on both feedwater quality and the type and If the system does not generate reagent water continuously,
condition of membranes used. recirculate the water through the ion exchanger. If resin regen-
Reverse osmosis membranes are available in both spiral-wound eration is economically attractive, use separate anion and cat-
and hollow-fiber configurations. The choice depends on the feed- ion resin beds, and position the anion exchanger downstream of
water’s characteristics and fouling potential. Obtain rejection data the cation exchanger to remove leachates from the cation resin.
for feedwater contaminants (levels of salt and impurities that will If the feedwater contains significant quantities of organic mat-
pass through the membranes compared to feedwater levels) at the ter, remove the organics first to minimize the potential for resin
https://doi.org/10.2105/SMWW.2882.010 1
1080 REAGENT WATER - C. Reagent Water Quality
fouling. Organics can be removed via prefiltration, distillation, to the solubility of the organics in water and the adsorption pro-
reverse osmosis, or adsorption. If using commercially prepared cess may be inadequate for removing low-molecular-weight, polar
resin columns, follow supplier’s recommendations for monitoring compounds. Performance differences among activated carbons are
QC of reagent water from specific equipment. attributable to the raw materials and activation procedures. Even
with an optimal activated carbon, proper performance will not be
4. Adsorption attained unless the column is sized to provide required face veloc-
ity and residence time at the maximum process flow rate. If using
In adsorption, water is fed into a reactor filled with an adsorbent commercial sorbent systems, follow the supplier’s recommended
material (typically, granular activated carbon, although some res- flow and QC steps.
ins and other manufactured adsorbents are used in specific appli- Using activated carbon may adversely affect the reagent water’s
cations). Chlorine and other organic impurities are drawn from resistivity. This effect may be controlled via reverse osmosis,
the water to the surface of the adsorbent. How well the process mixed resins, or special adsorbents. To minimize organic contam-
works depends on the organic contaminants involved, the activated ination, use mixtures of polishing resins with special carbons and
carbon’s physical characteristics, and the operating conditions. In additional treatment steps (e.g., reverse osmosis, natural carbons,
general, organics-adsorption efficiency is inversely proportional ultraviolet oxidation, or ultrafiltration).
https://doi.org/10.2105/SMWW.2882.010 2
1080 REAGENT WATER - C. Reagent Water Quality
Table 1080:2. Reagent Water Specifications the water from contamination (e.g., PTFE and glass for organics
Quality Parameter High Medium Low analysis or plastics for metals).
Resistivity, megohm-cm at 25 °C >10 >1 > 0.1
References
Conductivity, mmho/cm at 25 °C < 0.1 <1 <10
SiO2 (mg/L) < 0.05 < 0.1 <1
1. ASTM D-1193-06(2018). Standard specification for reagent water.
Annual Book of ASTM Standards; Vol 11.01. West Conshohocken
(PA): ASTM International; 2006.
The pH of high- or medium-quality water cannot be measured
2. ISO 3696:1987 (confirmed 2018). Water for analytical laboratory
accurately without contaminating the water, so measure other use: specification and test methods. Geneva, Switzerland: Interna-
constituents required for individual tests. tional Organization for Standardization; 1987.
High-quality water cannot be stored without degrading signifi- 3. CLSI GP40 (confirmed June 16, 2018). Preparation and testing of
cantly. Medium-quality water may be stored, but keep storage reagent water in the clinical laboratory: approved guidelines. 4th ed.
time to a minimum and make sure the quality remains consis- Annapolis Junction (MD): Clinical Laboratory Standards Institute;
tent with the intended use. Only store it in materials that protect 2006.