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Perchlorate in Sodium Hypochlorite

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Perchlorate in Sodium Hypochlorite emerging issues BY PETER GREINER, CLIF MCLELLAN, DALE BENNETT, AND ANGIE EWING Occurrence of perchlorate in sodium hypochlorite RESPONDING TO THE DETECTION erchlorate is both a synthetic and a naturally occurring chemical. Most of the perchlorate that is manufactured in the United States OF PERCHLORATE IN SODIUM is used as the primary ingredient of solid rocket propellant. Wastes HYPOCHLORITE BY THE from the manufacture and improper disposal of perchlorate-con- taining chemicals are increasingly being discovered in soil and water MASSACHUSETTS DEPARTMENT P (USEPA, 2007). OF ENVIRONMENTAL An additional source of perchlorate in drinking water has been found to occur through the use of sodium hypochlorite. The Massachusetts Department PROTECTION, of Environmental Protection (MDEP) has reported that significant levels of NSF INTERNATIONAL SURVEYED perchlorate can be detected in sodium hypochlorite samples that have aged for a few weeks (MDEP, 2005). Sodium hypochlorite as delivered to one utility FOR THE CONTAMINANT had a perchlorate concentration of 0.2 µg/L in the product, but the level of IN DRINKING WATER TREATMENT perchlorate rose to 6,750 µg/L after the product had aged for 26 days. CHEMICALS FROM PRODUCTION INVESTIGATION OF WATER TREATMENT CHEMICALS BEGAN IN 2005 FACILITIES ACROSS In 2005 NSF International began analyzing samples of drinking water treat- ment chemicals for the contaminant perchlorate. These samples were collected THE UNITED STATES as part of the annual testing requirement to support NSF certification of the AND CANADA. treatment chemical to NSF/American National Standards Institute Standard 60: Drinking Water Treatment Chemicals—Health Effects (NSF/ANSI, 2005). Samples collected included not only sodium hypochlorite but other types of chemicals as well. NSF 60 currently requires testing of sodium hypochlorite samples for regulated metals, volatile organic compounds, and bromate. NSF continued the investigation of sodium hypochlorite through July 2006, resulting in the analysis of more than 67% of NSF-certified manufac- turers across North America. The levels of perchlorate reported here reflect potential at-the-tap concentrations calculated in accordance with the proce- 68 NOVEMBER 2008 | JOURNAL AWWA • 100:11 | PEER-REVIEWED | GREINER ET AL 2008 © American Water Works Association Aliquots of the sodium hypochlorite samples collected at manufacturers’ facilities were placed in 40-mL amber glass vials and stored in the dark prior to testing. Perchlorate concentrations were determined by a liquid chromatography/mass spectrometry technique based on US Environmental Protection Agency method 331.0. duresdures in NNSFSF 60. TheseThese “normal-“normal- izization”ation” ccalculationsalculations pprojectroject popotentialtential at-tat-the-taphe-tap conceconcentrationsntrations by assumingassuming thethe treatment chemi-chemi- cacall iiss dosed aatt tthehe mmaximumaximum use llevelevel (MUL)(MUL) fforor wwhichhich it was certicerti-- ffied.ied. TypicaTypicallylly thethe MUL forfor so- ddiumium hhypochloriteypochlorite prproductsoducts is equivaequivalentlent to ddosingosing 10 mg/L ooff totatotall chlorinechlorine into water. AAlthoughlthough this concentration is sisignificantlygnificantly aboveb ththe US USE Environmental i t lP Pro- tection Agency (USEPA) maxi- mum residual disinfectant level goal of 4.0 mg/L, it provides a worst-case evaluation of the so - dium hypochlorite by accounting for other potential uses such as prechlorination during water treatment and use during shock chlorination of water systems. Perchlorate health effects. Per- chlorate affects the ability of the thyroid gland to take up iodine (ATSDR, 2005). Iodine is needed to make thyroid hormones that are released into the blood and regu- GREINER ET AL | PEER-REVIEWED | 100:11 • JOURNAL AWWA | NOVEMBER 2008 69 2008 © American Water Works Association late many body functions. Perchlo- final determination for perchlorate Laboratory analysis. The analysis rate is considered harmful to health after a 30-day public comment period. for perchlorate was performed when its inhibition of iodine uptake The agency also intends to issue a according to a modified USEPA is great enough to affect the thyroid. health advisory at the time it issues method 331.0, Determination of There is concern that hu man expo- the final regulatory determination in Perchlorate in Drinking Water by sure to higher amounts of perchlo- order to assist states with their local Liquid Chromatography Electro- rate for a long time may lower the response for perchlorate. spray Ionization Mass Spectrometry level of thyroid activity and lead to At the state level, perchlorate (USEPA, 2005). Method 331.0 is a hypothyroidism. Low levels of thy- guidance criteria of 14 µg/L in Ari- method for analyzing drinking roid hormones in the blood may zona, 5 µg/L in New York, and 1 water. All method requirements rel- adversely affect the skin, cardiovas- µg/L in Maryland and New Mexico evant to the analysis of sodium cular system, pulmonary system, have been adopted, along with hypochlorite rather than drinking kidneys, gastrointestinal tract, liver, action levels of 18 µg/L in New York water were included; the modifica- blood, neuromuscular system, ner- and Nevada and 4 µg/L in Texas tion of this method at NSF related to modification of the quality con- trol requirements. Method 331.0 allows for identi- fication by either tandem mass spec- trometry mode or single ion moni- erchlorate is considered harmful to health when its inhibition toring mode using dual ions (masses P 99 and 101). In this research, quan- of iodine uptake is great enough to affect the thyroid. tification was performed by internal standard calibration using the mass 101 ion. Results were reported in µg/L for liquid samples. In sodium hypochlorite, the average detection level for perchlorate was 250 µg/L. vous system, skeleton, male and (Bull et al, 2004). California has Approximately one third of the female reproductive systems, and established a perchlorate maximum samples tested were additionally numerous endocrine organs. Studies contaminant level (MCL) of 0.006 tested on multiple days to determine in animals have shown that the thy- mg/L (CDPH, 2007), and Massa- the rate of change in perchlorate con- roid gland is the main target of per- chusetts has established a perchlo- centration as the sodium hypochlo- chlorate toxicity. Animal studies rate MCL of 0.002 mg/L (MDEP, rite aged. Samples were maintained provided inconclusive results regard- 2006). For the purposes of estimat- in the dark and at room temperature ing effects of perchlorate on the ing the effect of perchlorate con- between analysis days. immune system. Perchlorate did not tamination, the current research affect reproduction in rats, accord- used the lowest of these values, in 164 CHEMICAL SAMPLES TESTED ing to one study. other words, 1 µg/L. Through July 2006, perchlorate Perchlorate regulation and guidance testing was performed on 164 sam- criteria. In October 2008 the USEPA SAMPLES NORMALLY COLLECTED ples of drinking water treatment announced a preliminary determina- DURING UNANNOUNCED AUDITS chemicals collected from 102 manu- tion on the regulation of perchlorate. TESTED FOR PERCHLORATE facturing locations. Of the 37 types After conducting an ex tensive review As part of NSF’s certification of chemicals tested, perchlorate was of scientific data re lated to the health program for drinking water treat- detected in only two: sodium effects of exposure to perchlorate ment chemicals, unannounced hydroxide and sodium hypochlorite from drinking water and other audits of manufacturing sites are (Table 1). sources, USEPA “. found that in performed annually, and samples of Of the 27 sodium hydroxide sam- over 99% of public drinking water certified treatment chemicals are ples, 22 (81%) had perchlorate levels systems, perchlorate was not at levels taken from recent production or reported as nondetectable; in the of public health concern. Therefore, retains. NSF used portions of these remaining five samples, perchlorate based on the Safe Drinking Water Act normally collected samples for this concentrations ranged from 0.01 to criteria, the agency determined there research on perchlorate. Once the 0.12 µg/L (Table 2). is not a ‘meaningful opportunity for samples were received at NSF, ali- The occurrence of perchlorate in health risk reduction’ through a quots were placed in 40-mL amber sodium hypochlorite was a more national drinking water regulation” glass vials and stored in the dark at common finding. Perchlorate was (USEPA, 2008). USEPA will make a room temperature before testing. detected in more than 91% of the 70 NOVEMBER 2008 | JOURNAL AWWA • 100:11 | PEER-REVIEWED | GREINER ET AL 2008 © American Water Works Association samples tested, at levels ranging from 0.03 to 29 µg/L. Table 3 TABLE 1 Summary of samples tested by chemical type groups the results by concentration range, including a running average Samples With of samples containing perchlorate at Samples Perchlorate levels less than or equal to the level With Perchlorate Detected Chemical Samples—n Detected—n % of perchlorate in the range. Of greater significance was the Aluminum chloride 1 correlation between the age of the Aluminum sulfate 2 sodium hypochlorite and the level of Ammonium hydroxide 3 perchlorate detected. Figure 1 shows Bentonite 1 the results of testing on samples Calcium hydroxide 1 with a known date of manufacture. Calcium hypochlorite 2 Results, plotted by sample age at the Calcium
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