The Shelf-Life of Sodium Hypochlorite Irrigating Solutions: Adrf Report
The Shelf-Life of Sodium Hypochlorite Irrigating Solutions: Adrf Report
Abstract INTRODUCTION
Background: Sodium hypochlorite (bleach) Biomechanical instrumentation and cleaning of root
solutions are widely used as irrigants in endodontics. canals require the use of an irrigant to suspend and
Their tendency to deteriorate is worsened by flush pulpal and dentinal debris from root canals.1
environmental influences which could cause loss of Ideally, an endodontic irrigant should be sterile and
available chlorine content.
Methods: This study measured the loss of available should also be capable of destroying the micro-
chlorine concentration in a range of sodium organisms found in a necrotic pulp, as well as
hypochlorite solutions under conditions which dissolving both vital and necrotic pulpal tissue.2-4
mimic clinical usage and storage. Domestic bleach, Sodium hypochlorite solutions, which are bactericidal,
both undiluted and diluted with demineralised water virucidal and which dissolve protein, have been widely
or hard water, was tested, along with Milton, for
used for this purpose.5-7 The concentration of sodium
initial concentration of available chlorine, and then
retested after varying periods and modes of storage hypochlorite solutions used in endodontics may vary
to measure loss of chlorine concentration. The types from 0.5-5.25 per cent available chlorine.8 While
of storage were: (1) in closed plastic bottles which sodium hypochlorite may be prepared and packaged
were opened daily and agitated; (2) in open plastic commercially for therapeutic use,1 it is common in
bottles; (3) in syringes exposed to sunlight; (4) in many countries for domestic bleach (diluted or
syringes kept in the dark; (5) in open stainless steel
undiluted) to be used as an endodontic irrigant.8
bowls; (6) in closed stainless steel bowls; and (7)
when heated to 50°C. Not all solutions were tested Sodium hypochlorite is a strong oxidising agent.9 The
under all storage conditions. level of available chlorine is the critical factor affecting
Results: Of the solutions opened daily, undiluted the activity of sodium hypochlorite solutions.5,10 These
domestic bleach was the most stable and Milton was solutions are unstable.11 Available chlorine
the least stable. Initially, diluted bleach left open
concentration deteriorates with time, exposure to
deteriorated rapidly but deterioration slowed with
time. Solutions in syringes exposed to sunlight light5,12 and heat8,13 and on contact with air,5,12 metals,
showed the most rapid loss of chlorine content. metallic ions10 and organic materials.1 While Velvart14
Heated bleach lost nearly 5 per cent of its strength in concluded that cold storage did not appear to improve
six hours. Diluted bleach surprisingly, increased its the shelf-life of two per cent solutions, other authors8,11
chlorine concentration in open bowls probably due demonstrated much better shelf-life under refrigeration,
to evaporation of water. Dilution of bleach with
and concluded dilute solutions were more stable than
hard tap water did not significantly affect shelf-life.
Preloading of diluted bleach into syringes appears to more concentrated solutions. While the bactericidal
be a sound technique if the syringes are stored away activity is greater at pH values as low as 6, high pH
from light. levels are necessary for effective shelf-life.6,11 Sodium
Conclusions: This study reinforces the need for hydroxide is usually present in the solutions to
sodium hypochlorite to be stored in closed opaque enhance alkalinity.
containers. Constant opening of containers appears
to cause greater loss in chlorine concentration of While the individual influences of environmental
diluted bleach solutions, perhaps because a lower factors on the stability of sodium hypochlorite have
concentration of sodium hydroxide allows the pH to been well documented, the influence of many of the
drop more rapidly. factors which are likely to be encountered in clinical
Key words: Sodium hypochlorite, domestic bleach, endodontic practice in combination have not been
endodontics, shelf-life, clinical usage, open containers, examined. The most pertinent of these influences are
syringes. combinations of time, temperature and exposure to
(Received for publication October 2000. Revised November light and air. In view of the recorded instability of
2000. Accepted for publication December 2000.) sodium hypochlorite solutions and of the wide range of
potential storage conditions and methods of dispensing
*General practitioner, Kingaroy.
†Specialist endodontist, Brisbane.
these solutions in different dental practices, further
‡Statistical consultant, The University of Queensland. examination of shelf-life under combinations of storage
Australian Dental Journal 2001;46:4. 269
and dispensing conditions which could accelerate the Table 1. Analysis of water from Kingaroy domestic
loss of available chlorine concentration was considered supply used to dilute domestic bleach.*
warranted. Contents Concentration mg/L
The activity of sodium hypochlorite solutions can be Cations
assessed by determining the amount of available Sodium 335
Potassium 12
chlorine in each solution. There are a number of Calcium 105
methods to measure available chlorine, including tissue Magnesium 130
solubility;10 N-diethyl-p-phenylenediamine ferrous Hydrogen 0
ammonium sulphate analysis;5 titration against sodium Anions
arsenite;11 and iodometric titration with a variety of Bicarbonate 125
end-point detection procedures, which include titration Carbonate 1.6
Hydroxide 0
against sodium thiosulphate and amperometric Chloride 980
titration against phenylarsine.15 While the accuracy of Fluoride 0.1
iodometric titration against sodium thiosulphate has Nitrate 3.7
Sulphate 46
been questioned,11 because breakdown products such as
chlorates and chlorites could potentially give artificially Other dissolved elements
high readings, it is the simplest and most widely used Iron <0.02
Manganese 0.06
test for available chlorine; does not have the disposal Zinc <0.02
problems or toxicity of arsenic compounds;15 and was Aluminium <0.05
used in this study. Boron 0.1
Copper <0.05
This study examined hypochlorite solutions
*Collected 28th August 1995 – tested April 1997 by Scientific
commonly used for endodontic irrigation in Australia. Services section of Queensland Health.
Solutions assessed included an infant sanitiser and a
common brand of domestic bleach, both undiluted and
diluted. Changes in available chlorine concentrations period. The solutions in syringes were treated
were investigated when the solutions were exposed to differently – the contents of six syringes were combined
combinations of environmental and storage variables and stirred to make a solution from which three
commonly found in dental practices. titrations were carried out at each test period. Solutions
in syringes exposed to sunlight were titrated by a single
M AT E R I A L S A N D M E T H O D S operator and all other titrations were carried out by
Sodium hypochlorite solutions teams of two operators, each making independent
Milton (Proctor & Gamble Australia, Parramatta, readings of the titration results. The 10 solutions were
NSW) (1 per cent w/v) and Sno-Wite (Kiwi Australia, tested immediately upon preparation and at varying
Clayton South, Vic) (4 per cent w/v) were used as the intervals depending on the storage conditions.
sources of sodium hypochlorite for this study. Milton
was used in the undiluted form only and Sno-Wite was Available chlorine
also used undiluted or diluted to 1 per cent w/v. To test the effect of storage conditions on shelf-life,
Sno-Wite solutions were diluted to one per cent w/v
Titrations with both demineralised water and hard tapwater, then
The level of available chlorine was assessed initially stored in the following manner:
and at each test period, using Australian Standard
1087.16 This test was developed for sodium (1) In one-litre bottles which were opened daily
hypochlorite solutions used in the dairy industry and Plastic one-litre bottles were half-filled with dilute
involved addition of potassium iodide to a prepared Sno-Wite, then tightly capped, wrapped in aluminium
sodium hypochlorite solution, with subsequent foil to help exclude light and placed in a lightproof box.
addition of acetic acid. Available chlorine oxidised the Each bottle was opened daily five days a week, agitated
iodide ions to produce iodine which turned the solution briefly then recapped after 10 minutes. Available
brown. The resulting solution was then titrated against chlorine levels were tested at varying intervals over
a standard sodium thiosulphate solution (0.1 eight months. The one per cent w/v solutions were
mole/litre) until the colour just disappeared. The stored in numbered containers. The titrating staff were
concentration of available chlorine was given by the not aware of the identity of solutions being tested.
following equation: per cent available chlorine equals
VC3.546, where V equals the volume of sodium (2) In open containers
thiosulphate used in millilitres and C equals the In this segment of the study, an identical solution to
concentration of the standard sodium thiosulphate that prepared in (1) above was prepared and placed in
solution in moles/litre. individual one-litre bottles which were wrapped in
For all solutions except those in syringes, three aluminium foil and stored in a lightproof, ventilated
samples were prepared and three titrations were box in a photographic darkroom, with the bottles
performed on each sample at the end of each storage remaining uncapped.
270 Australian Dental Journal 2001;46:4.
Table 2. Sodium hypochlorite test solutions and details of conditions of storage and container type.
Parent Diluent Nominal concentration of Storage Container Opened Light Container
solution used test solution* temperature capped daily exposure type
Milton Nil 1 Air conditioned Yes Yes Dark 1L plastic
Sno-Wite Nil 4 Air conditioned Yes Yes Dark 1L plastic
Sno-Wite Nil 4 50°C No Open Ambient 100ml glass
Sno-Wite Demin 1 Air conditioned Yes No Sunlight 5ml syringe
Sno-Wite Demin 1 Air conditioned Yes No Dark 5ml syringe
Sno-Wite Demin 1 Air conditioned No Open Dark 1L plastic
Sno-Wite Demin 1 Air conditioned No Open Ambient Stainless bowl
Sno-Wite Demin 1 Air conditioned Yes No Ambient Stainless bowl
Sno-Wite Hard 1 Air conditioned Yes Yes Dark 1L plastic
Sno-Wite Demin 1 Air conditioned Yes Yes Dark 1L plastic
*Per cent available chlorine. Demin – demineralised water. Hard – hard water from Table 1. Sunlight – indirect sunlight. Ambient – sunlight from
windows plus fluorescent lights.
(3) Using hard tapwater for dilution tested were tabulated according to the parent
These solutions were prepared and stored as in (1) hypochlorite solution; type of water used for dilution
above, but the Sno-Wite was diluted with tapwater (if any); storage temperature; whether the container
obtained from the Kingaroy reticulated supply during a was left open, covered or opened daily; the nature of
period of prolonged drought. Detailed analysis of this exposure to light; and the type of container used (Table
water is provided in Table 1. 2). Changes in chlorine concentration over time were
graphed for all solutions, with chlorine content
(4) In syringes exposed to sunlight expressed as a percentage of the initial available chlo-
Diluted Sno-Wite was pre-loaded into 5mL disposable rine concentration.
syringes (Becton Dickinson Medical, Singapore) with
one inch 30 gauge needles attached. The syringes were pH of solutions stored for eight months
stored on a window ledge in indirect sunlight. Solutions The pH of all solutions tested over eight months was
were tested after 6, 15, 23 and 30 days. measured on the same day as the final titrations, using
an appropriately calibrated Activon (Activon,
(5) In syringes stored in the dark Gladesville, NSW) model 109 pH meter, and tabulated
Syringes and solution identical to (4) above, were to compare them statistically with the final
stored in a closed cardboard box, in air-conditioned concentrations of these solutions (Table 3).
premises, and tested after 42 and 98 days.
Statistics
(6) In stainless steel bowls Statistical methods used to analyse the data varied
In this part of the study, solutions of diluted Sno- for different segments of the study. These are specified
Wite were placed into stainless steel bowls, both open in reporting the results. For clarity in detailing the
to the atmosphere and covered with polythene cling- preparation and storage of test solutions, textual
wrap to exclude air. The solutions were stirred prior to divisions used in the results section vary slightly from
sampling and testing, which was carried out after six those used in (1) to (8) above.
and five hours respectively.
R E S U LT S
Undiluted Milton and Sno-Wite were also tested in Solutions stored for eight months
the following manner: Changes in mean concentration of the five solutions
stored over approximately eight months are illustrated
(7) In containers which were opened and agitated daily in Fig 1. Undiluted Sno-Wite was the most stable
The parent solutions of these two products were solution (p<0.05), losing just over 10 per cent of its
stored in identical one-litre plastic bottles, in the same original strength over the experimental period.
lightproof box and subjected to the same regime of However, the stability of Sno-Wite was not significantly
daily opening and agitation as in (1) above, and also different from the other solutions opened and agitated
tested over eight months. daily at the end of the first and third months (p>0.05).
Milton was the least stable solution, deteriorating over
(8) After storage at 50°C the eight month period to just over 11 per cent of its
Four per cent w/v Sno-Wite was placed in 100mL initial concentration (mean concentration in nine
measuring cylinders immersed in water at a constant samples 11.043 per cent with a standard error of
50°C. The cylinders were loosely covered to prevent 0.530). The other three solutions were not significantly
dilution by splash from the water bath and the contents different in mean concentration percentage after eight
evaluated after five hours. months (p>0.05), their mean values ranging between
The five test solutions in (1), (2), (3), and (7) above, 41.8 (standard error 3.906) and 47.8 per cent (standard
were analysed at 35, 98 and 238 days. All solutions error 9.463). The Sno-Wite diluted with hard water
Australian Dental Journal 2001;46:4. 271
Table 3. pH and concentration of sodium
hypochlorite solutions after storage for eight months
while opened daily or left permanently open.
Solutions Average concentrations % Average pH
Milton 0.125 8.533
Hard 0.415 9.363
Demin 0.474 9.507
Sno-Wite 3.554 12.517
Open 0.465 9.657
Hard – Sno-Wite diluted with hard water. Demin – Sno-Wite diluted
with demineralised water. Open – Sno-Wite diluted with
demineralised water and left permanently open.
Fig 4. Rust formation after seven days in syringes loaded with Milton
and stored in the dark. Fig 4a shows demonstrable rust formation in
drops of Milton trapped in needle sheath of syringe. In Fig 4b, the
lumen of the 30 gauge needle appears completely occluded by rust.