US5211855A

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United States Patent ps5
Antelman

NN

US005211855A

il] Patent Number: 5,211,855
[45] Date of Patent: * May 18, 1993

[54] METHOD OF TREATING WATER
EMPLOYING TETRASILVER TETROXIDE
CRYSTALS

[75] Inventor: Marvin S, Antelman, Rehovot, Israel

[73] Assignee: N. Jonas & Co., Inc., Bensalem, Pa.

[*] Notice: The portion of the term of this patent
subsequent to May 21, 2008 has been
disclaimed.

[21] Appl. No.: 825,623

[22] Filed: Jan, 24, 1992

[51] Int. CLS w. CO2F 1/50

[52], U.S. Cl. 210/758; 210/764;

422/28; 424/618
[58] Field of Search ..................... 210/169, 198.1, 501,
210/764, 758; 422/19, 28; 424/601, 602, 604,
618, 709; 514/495; 423/42, 45, 544, 604
[56] References Cited
U.S. PATENT DOCUMENTS

4,055,655 10/1977 Maurer et al.

514/495

4,092,245 5/1978 Franks et al. 210/169
4,492,618 1/1985 Eder ... 210/764
5,017,295 5/1991 Antelman .. 210/764

5,073,382 12/1991 Antelman . 210/169

5,078,902 1/1992 Antelman . 210/764
5,089,275 2/1992 Antelman .. 210/169
5,098,582 3/1992 Antelman . 210/764

OTHER PUBLICATIONS

Hawley’s Condensed Chemical Dictionary, 11th ed, p.
699 (definition of Ligand).

Hammer & Kleinberg Inorganic Synthesis vol. IV, p.
12.

J. Servian & H. Buenafama, Inorg. NUC. Letters 5, 337.

Primary Examiner—Peter Hruskoci
Assistant Examiner—Robert James Popovics
Attorney, Agent, or Firm—Salter, Michaelson & Benson

157] ABSTRACT

A novel molecular scale device is described which is
bactericidal, fungicidal and algicidal. The antipatho-
genic properties of the device are attributed to electron
activity indigenous to diamagnetic semiconducting
crystals of tetrasilver tetroxide (Ag4O4) which contains
two monovalent and two trivalent silver ions in each
molecular crystal. When the crystals are activated with
an oxidizing agent, they release electrons equivalert to
6.4X 10-19 watts per molecule which in effect electro-
cute pathogens. A multitude of these devices are effec-
tive at such low concentrations as 0.3 PPM where they
car kill 100% of 100 K/cc Streptococcus faecalis, and
E. coli colonies in three minutes meeting the ten-minute
EPA criteria of 100% kills within ten minutes for swim-
ming pool and hot-tub applications. The devices can be
used in utilitarian bodies of water, such as municipal and
industrial water reservoirs.

4 Claims, 1 Drawing Sheet

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METHOD OF TREATING WATER EMPLOYING .
TETRASILVER TETROXIDE CRYSTALS

BACKGROUND OF THE INVENTION

The present invention relates to the employment of
molecular crystals as bactericidal, viricidal and algicidal
devices, but more particularly to the molecular crystal
semiconductor tetrasilver tetroxide Ag4O4 which has
two trivalent and two monovalent silver atoms per
molecule, and which through this structural configura-
tion enables electronic activity on a molecular scale
capable of killing algae and bacteria via the same mech-
anism as macroscale electron generators. The concept
of molecular scale semiconductor devices for the stor-
age of information has been the subject of much activity
in recent years so that the concept of a molecular scale
device performing such functions as storing information
or acting as resistors, capacitors or photovoltaic devices
is well accepted. The molecular device of this invention
is a multivalent silver diamagnetic semiconductor. The
bactericidal activity of soluble divalent silver (Ag II)
complex bactericides is the subject of U.S. Pat. No.
5,017,295 of the present inventor. The inventor has also
been granted U.S. Pat. Nos. 5,078,902, 5,073,382,
5,089,275, and 5,098,582, which all deal with Ag II
bactericides but more particularly with (respectively)
halides, alkaline pH, stabilized complexes and the diva-
lent oxide. It is U.S. Pat. No. 5,098,582, and its perfec-
tion that has led to the present invention. This: patent
designated AgO as divalent silver oxide, the popular
name of the compound. Indeed, the Merck Index (11th
Edition) designates the oxide as silver(I) oxide (AgO)
(entry 8469). However, it also states that it is actually a
silver(I)-silver(III) oxide with a molecular weight of
123.88. After filing my patent application, a comprehen-
sive examination was begun of information relating to
the structure of this oxide. Further investigation of the
scientific literature revealed that said oxide was actually
on a molecular level AgaO4 where one pair of silver
ions in the molecule was trivalent and another pair was
monovalent. Said oxide is actually on a molecular level
AgsO4 where one pair of silver ions in the molecule is
trivalent and another pair is monovalent.

While the formula AgO accurately designates the
silver:oxygen ratio, the molecular weight of the com-
pound is actually 495.52. Further elucidation of the
molecule’s electromagnetic properties revealed that it is
a diamagnetic semiconductor. The structure is electron-
ically active because of the trivalent sp? electron config-
uration disparity of the electrons within the crystal. The
oxide as presented in my patent was actually capable of
killing 100% of standardized E. coli and Strep. faecalis
colonies in less than five minutes at concentratiors of 0.5
PPM. My independent evaluations of this oxide in areas
unrelated to water treatment resulted in the “molecular
device” concept which was substantiated by submission
of the oxide for testing with a preferred embodiment of
the invention (10 PPM of sodium persulfate) at an Envi-
ronmental Protection Agency (EPA) certified labora-
tory which revealed that 0.5 PPM of oxide only yielded
0.003 PPM of silver in solution, a silver. concentration
entirely too low to cause this level of bactericidal activ-
ity. Indeed, the killing of the bacteria was analogous to
that obtained by electron generating devices utilized in
swimming pools or water towers for killing bacteria. It
was therefore postulated that the oxide efficacy at low
concentrations could only be attributed to regarding

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each oxide molecule as a device. Further testing was
continued on algae and viruses. The accumulated data
of efficacy at low concentrations, coupled together
with a reinterpretation of silver oxide efficacy, has led
to the final development of this invention, namely, a
molecular device for killing algae, bacteria and viruses
in utilitarian water bodies, such as swimming pools.

OBJECTS OF THE INVENTION

The main object of this invention is to provide for a
molecular scale device of a single tetrasilver tetroxide
semiconductor crystal capable of killing viruses, bac-
teria, and algae when operating in conjunction with
other such devices.

Another object of the invention is to provide for a
device which is so small that several thousand trillion
can be added to a water supply to perform their effec-
tive functions and still be effective at concentrations of
the devices in said supply not exceeding one part per
million.

Still another object of the invention is to provide for
a device which will perform the aforementioned anti-
pathogenic functions without polluting the water
supplies it is intended to purify, such as swimming
pools, industrial cooling towers, hot tubs and municipal
water supplies.

Still another object of the invention is to provide for
a device which can be employed in swimming pools,
hot tubs and other environments for these aforemen-
tioned functions in the presence of humans, without
causing them respiratory and eye irritations and other
nuisance effects characteristic of active sanitizers based
on halogens such as chlorine, one such nuisance affect
being the deterioration of bathing suits.

Other objects and features of the present invention
will become apparent to those skilled in the art when
the present invention is considered in view of the ac-
companying examples. It should, of course, be recog-
nized that the accompanying examples illustrate pre-
ferred embodiments of the present invention and are not
intended as a means of defining the limits and scope of
the present invention.

SUMMARY OF THE INVENTION

This invention relates to a molecular scale device
capable of destroying gram positive and gram negative
bacteria as well as viruses and algae. Said molecular
scale device consists of a single crystal of tetrasilver
tetroxide. Several hundred thousand trillion of these
devices may be employed in concert for their bacteri-
cidal, viricidal, and algicidal properties and applied to
industrial cooling towers, swimming pools, hot tubs,
and municipal water supplies.

- The molecular crystals which are the subject of this
invention are commercially available and can be pre-
pared by reacting silver nitrate with sodium or potas-
sium peroxydisulfate according to the following equa-
tion:

44gNO3+2Na2S20z+8NaOH=AgsOu+4Nap.
504+4NaNO3+4H20

The oxide lattice represented by the formula Ag4Og is
depicted in the Drawing FIG. 1. It is a semiconducting
electron active diamagnetic crystal containing two
monovalent and two trivalent silver ions in combination
with four oxygen atoms. The distance between the
Ag(III)-O Ag(1)O units equals 2.1 A. Ag(III)-Ag(III)-

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=Ag(I)-Ag(I)=3.28A and Ag(I)-Ag(III=3.19 A.
Each trivalent silver ion is coordinated via dsp electron
bonds to 4 oxygen atoms. The depiction of this lattice is
based on several literature references relating to crystal-
lographic studies. Exemplary of this literature are J. A.
McMillan’s studies appearing in Inorganic Chemistry
13,28 (1960); Nature vol. 195 No. 4841 (1962), and
Chemical Reviews 1962, 62,65. Alvin J. Salkind eluci-
dated studies involving neutron diffraction with his
coworkers (J. Ricerca Sci, 30, 1034 1960) proving the
Ag(III)/Ag(I) nature of this molecule and states in his
classic entitled Alkaline Storage Batteries (Wiley 1969),
coauthored with S. Uno Falk, that the formula is de-
picted by Ag4Ox (page 156).

That same year a scientific communication appeared
in Inorganic Nuclear Chemistry Letters (5,337) authored
by J. Servian and H. Buenafama which maintained that
their neutron diffraction studies also confirmed the
tetroxide lattice and the presence cf Ag(III) and Ag(I)
bonds in the lattice, a conclusion also reported previ-
ously by Naray-Szahn and Argay as a result of their
x-ray diffraction studies (Acta Cryst. 1965, 19,180). Thus
the effects of this invention can be explained in terms of
these structural elucidations, namely, that the single
molecular semiconductor crystal which inevitably must
be electronically active exchanging two electrons per
crystals between its mono and trivalent bonds is in real-
ity a device which kills pathogens in the same manner as
electrically active large-scale devices utilized in water
supplies.

When the tetroxide crystals are utilized to destroy
pathogens, they will not do so unless activated by an
oxidizing agent. This is analogous to the behavior of
single semiconducting photovoltaic molecular devices
such as copper indium selenide whose surfaces must be
“etched” in order to activate the photovoltaic activity,
ie., for light to facilitate the release of electrons from
the molecule. The tetroxide was activated by persul-
fates. It was found that when the persulfates were tested
as a control by themselves, they failed to exhibit any
unilateral antipathogenic activity at the optimum level
selected of 10 PPM. The persulfates evaluated varied
from OXONE (Registered Trademark Du Pont Com-
pany) brand potassium monopersulfate to alkali perox-
ydisulfates.

DESCRIPTION OF THE DRAWING

In the drawing which illustrates the best mode pres-
ently contemplated for carrying out the present inven-
tion:

FIG. 1 is a diagrammatic view showing the molecular
crystal Ag4Og attacking a pathogenic bacillus.

DESCRIPTION OF THE INVENTION

Turning now to Drawing FIG. 1 depicting the crys-
tal lattice of Ag4Oq, the device operates by transferring
electrons from the monovalent silver ions 10 to the
trivalent silver ions 11 in the crystal 20 through the
aqueous media in which it is immersed and which con-
ducts electrons depicted by the path 12, contributing to
the death of pathogen 13 with electrons 14, traversing
the cell membrane surface 15, said pathogen being
“electrocuted” by not only these electrons but by oth-
ers: 16 and 17 following paths 18, and 19 emanating
from other molecular devices in the vicinity of the
pathogen. Drawing FIG. 1 exaggerates the size of the
silver oxide molecular device with respect to that of a
microorganism for depiction purposes only. The device

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is attracted to the cell membrane surface 15 by powerful
covalent bonding forces 21 caused by the well-known
affinity of silver to certain elements present in the mem-
brane, such as sulfur and nitrogen.

The electron transfer can be depicted by the follow-
ing half reactions in which the monovalent silver ion
Joses an electron and the trivalent silver gains one as
follows:

Agt —e=Agt2

Agt3iemAgt?
The molecular crystal then will become stabilized with
each silver ion having a divalent charge.

The molecular device was evaluated in concentra-
tions ranging from 0.5 to 5.0 PPM on mixed gram posi-
tive and gram negative cultures and mixed coliforms for
evaluation in conjunction with EPA protocols for
swimming pools in the presence of 10 PPM sodium
persulfate. It killed 100% of colonies of Streptococcus
faecalis and E. coli within three minutes at 0.5 PPM.
The EPA requirement is within ten minutes. The col-
ony concentrations were 100,000/cc.

In order to consider the possibility that silver ions
escaping the crystal device may have had an influence
on the bactericidal properties of the device especially if
those silver ions were of a higher valence state facili-
tated by the persulfate according to the reaction:

AgO+ H20=Agt?+420H—

Ag4O4 crystals were sent to an independent EPA certi-
fied testing laboratory together with sodium persulfate
with specific instructions to prepare Ag4O4 suspensions
in 10 PPM persulfate at various concentrations. The
preparations were made in one-liter volumetric flasks
utilizing 0.5 mg and other concentrations /L of AgsO4,
where the concentration of mg. per liter equals parts per
million of the oxide. After vigorous mixing of the oxide
crystals in the flasks, the solutions were allowed to
remain undisturbed for 24 hours. After that time period
the supernatant liquid was analyzed for silver utilizing
atomic absorption spectroscopy with inductively cou-
pled plasma. At 0.5 PPM Ag4Os there was only silver
found equivalent to 0.003 PPM. This concentration is so
low that even if it were speculated that the ions were in
a higher valence state, they could never even then be
considered bactericidal. Indeed, the inventor’s U.S. Pat.
No. 5,017,295 involving divalent silver bactericides
claims these compounds at the lowest silver ion concen-
tration of 0.5 PPM.

If we are to consider one molecular device in opera-
tion, then each molecule would release two electrons
having each a charge of 4.8< 10-10 e.s.u. equivalent to
approximately 1.6 10—-!9 coulombs. The EMF given
in my Encyclopedia of Chemical Electrode Potentials
(Plenum 1982), page 88, for the oxidation of Ag(I) to
Ag(I}) is 1.98 volts which approximates 2.0 V. The total
power output per.device can be calculated in watts by
multiplying the power output for each electron by 2.
Since power is the product of the potential times the
charge, P=EI; for each electron it would be

2.0X 1.6 10~19=3.2x 10-9 warts

From this, and using Avogadro’s number, we can calcu-
late that the power flux of one liter of solution contain-
ing 0.5 PPM of devices would be 0.064 watts. Since the
electronic charges of the devices are directly propor-

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tional to the number of devices in solution, i.e., the
concentration of the oxide in the solution, we can arbi-
trarily assign our own device power. flux constant
which can be used to gauge the concentrations of the
devices required in order to kill particular organisms in
specific environments. I have found the following for-
mula useful for this purpose:

Power Flux=EMF generated per
molecule X Concentration x 5

(the EMF being 4.0 volts per molecular device times
the concentration in PPM). Utilizing this formula, the
power flux to effectuate 100% kills for E. coli and Strep-
tococeus faecalis is equal to 6.0.

Tests were conducted to see whether the molecular
crystals posed any harm to the human body. Accord-
ingly, a 3% concentrate of the crystals was prepared for
a series of evaluations.

The first evaluation met the requirements of Code of
Federal Regulations (CFR) 40 part 160 which consisted
of determining the single dose toxicity in rats or LDso.
All the animals survived so that the LDso was greater
than 5.0 g./Kg. This was true for concentrations of
crystals of a magnitude of 6-60,000 times the actual
concentrations that would be used in its utilization. This
test classified the device as a category IV substance
according to EPA protocols.

The second evaluation was for acute dermal toxicity
in rabbits. The protocol, 40 CFR 158.135, 81-2, was to
determine the LDso for dermal application. All animals
survived the maximum dose 2.0 g/Kg,, classifying the

crystals as category III with a dermal LDspo greater
than 2000 mg/Kg.

The third evaluation, entitled “Primary Dermal Irri-
tation in Albino Rabbits”, conformed to 40 CFR 160. It
consisted of exposing the rabbits for prolonged periods
of time and observing edema, erythema, ulceration,
necrosis and any other evidence of dermal reactions or
tissue destruction. There were none, classifying the
crystal concentrate as a category IV dermal agent by
EPA criteria.

The fourth evaluation dealt with primary eye irrita-
tion. This also was in conformity with 40 CFR part 160.
There was absolutely no eye irritation when the crystal
concentrate was applied, classifying it as a category IV
substance with regard to eye effects according to EPA
criteria.

The concentrate submitted for these evaluations, i.e.,
the 3% suspension of crystals, represented a concentra-
tion 1.50% times as great as the end product intended
for commercialization, namely, a 2% suspersion of sil-
ver oxide crystals.

The crystals were also evaluated by monitoring their
performance over a period cf time at various concentra-
tions. Periodically, water samples were taken and
shipped in a refrigerated state for bacterial counts. Ac-
cordingly, the device performed in concert with its
attendant devices in full conformity with the ultimate
objects of this invention.

Other objects and features of the present invention
will become apparent to those skilled in the art when
the present invention is considered in view of the ac-
companying examples. It should, of course, be recog-
nized that the accompanying examples illustrate pre-
ferred embodiments of the present invention and are not
intended as a means of defining the limits and scope of
the present invention.

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EXAMPLE 1

Tetrasilver tetroxide (Ag4O,) crystals were prepared
by modifying the procedure described by Hammer and
Kleinberg in Inorganic Syntheses (IV,12). A stock solu-
tion was prepared by dissolving 24.0 grams of potassium
peroxydisulfate in distilled water and subsequently add-
ing to this 24.0 of sodium hydroxide and then diluting
the entire solution with said water to a final volume of
500 ml. Into 20 ml. vials were weighed aliquots of silver
nitrate containing 1.0 g. of silver. Now 50 ml. of the
aforementioned stock solution were heated in a 100 ml.
beaker, and the contents of one of the vials was added to
the solution upon attaining a temperature of 85° C. The
beaker was then maintained at 90° C. for 15 minutes.
The resulting deep black oxide obtained consisting of
molecular crystal devices was washed and decanted
four times with distilled water in order to remove impu-
tities. The purified material was collected for further
evaluation and comparison with commercial material.
The commercial material was purchased from Johnson
Matthey’s Catalog Chemicals Division of the Aesar
Group of Ward Hill, Massachusetts, under product
code 11607 and generically listed in its materials Safety
Data Sheet as both silver peroxide and silver suboxide,
having a purity of 99.9%.

Both the prepared and commercial device crystals
were submitted for bactericidal evaluation following
“good laboratory practice” regulations as set forth in
Federal Regulations (FIFRA and ffdca/40 CFR 160,
May 2, 1984). The protocols consisted of exposures to
Streptococcus faecalis, a gram positive pathogenic ba-
cillus utilizing AOAC (15th) 1990:965:13: at colony
densities of 100 000 colonies/cc. and two exposure
times of five and ten minutes. The devices were tested at
concentrations of 0.3, 0.5 and 1.0 PPM in distilled water
adjusted to pH=7.5 and containing Oxone (Registered
Trademark Du Pont Company), which is potassium
monopersulfate at a level of 10 PPM. The evaluations
were repeated at the same persulfate concentration
utilizing commercial grade sodium persulfate manufac-
tured by FMC. 100% kills were actually obtained after
three minutes at all the aforementioned device concen-
trations, there being actually zero colonies at the 0.5 and
1.0 PPM levels after five minutes and at the 0.3 PPM
level after ten minutes. Analogous testing employing
the same colony density of the gram negative bacillus E.
coli were carried out. The same results were obtained.
EPA criteria require that 100% kills be obtained within
ten minutes for a substance to meet EPA criteria for
swimming pool utilizatior. In this case, the devices at
0.3 PPM, equivalent to approximately 360,000 trillion
devices, were able to far exceed EPA criteria for sani-
tizing a swimming pool. '

EXAMPLE 2

Commercial grade silver oxide prepared according to
the method of Example 1, but which is actually the
tetrasilver tetroxide molecular devices were tested ina
swimming pool under actual-use conditions. The swim-
ming pool contained approximately 27,000 gallons of
water. The level of the device crystal concentration
was maintained at 1.0-1.5 PPM. The swimming pool
was periodically monitored by removing water samples
for pH, silver calcium, algae and bacteria. The swim-
ming pool was utilized on a daily basis over a period of
six weeks by an average number of four people per day.
The pool was made up fresh with a fresh coating of

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plaster. The initial pH was 9.7. By the end of the first
week, the pH dropped to 8.2. Thereafter the average
daily pH of the pool was 7.8. The calcium level of the
pool was allowed to rise slowly from an initial 100 PPM
to 220-240 PPM. Without any new additions of silver to
the solution of the initial 1.5 PPM molecular crystal
concentration, the pool had zero bacteria and zero al-
gae. Other extraneous factors were also monitored,
such as copper (0.1-0.2 PPM) and iron (initial .0 aver-
age .05 PPM), which did not affect the results.

EXAMPLE 3

Tests were performed on residual silver concentra-
tion of device crystals in water to see whether the de-
vices could be used to treat municipal drinking water
supplies since the devices had proven to be antipatho-
genic at 0.3 PPM according to Example 1. Now there is
no adverse health effect for silver at the present time
according to the EPA, and it has been dropped from the
1991 pollutants list according to 56 FR 1470 p.7. A
secondary maximum contaminant level for drinking
water involving silver was proposed in 1989 (54 FR
22062), May 22, 1989) of 0.1 PPM. The oxidizing agent
to activate the crystals for water supplies would be
OXONE (Registered Trademark Du Pont Company)
or hydrogen peroxide. Accordingly, brand potassium
monopersulfate samples of commercial oxide devices of
Aesar origin as heretofore described were sent to an
EPA certified laboratory for evaluation. The laboratory
prepared samples of the devices at concentrations of
0.5, 1.0, 2.0, 5.0 and 10.0 PPM in 10 PPM sodium persul-
fate solution. The solutions were allowed to stand for 24
hours, after which the supernatant liquid was tested for
residual silver content by atomic absorption spectros-
copy using inductively coupled plasma as the excitation
source. The respective amounts of silver found in the
supernatant liquid were respectively 0.003, 0.13, 0.52
and 0.94 PPM. This means that at a concentration of
nearly double the pathogenic inhibition requirement
level that the secondary silver allowance of 0.1 PPM
was hardly reached, which qualifies the devices for
drinking water.

EXAMPLE 4

The devices were tested against AIDS virus. The
protocol used was that of the Ministry of Health of the
State of Israel at their Virology Laboratory located at
Tel HaShomer, Israel. AIDS viruses which had been
grown in vitro in a tissue culture were isolated and
exposed to the devices at device concentrations of 0.05,
1,0, 2.0, 3.0, 5.0 and 10.0 PPM. There was no evidence
of AIDS suppression at all until the concentrations
reached 5.0 and 10.0 PPM. At 5.0 PPM, 60% of the
viruses were killed. AT 10.0 PPM, 75% of the viruses
were killed. Extrapolation of this data reveals that at

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18.0 PPM there would be total suppression of the virus.
These test results indicate that the devices are capable
of being used to destroy viruses in applications involv-
ing the proliferation and transmittal of the AIDS virus
outside of the human body as in cold sterilization.

EXAMPLE 5

An ATTC strain of Chorella was grown in nutrient
Medium 866 broth under the required lighting. When
optimal growth was reached, the number of organisms
per ml. were determined by microscopic count and then
subcultured. The molecular crystal devices were ap-
plied to the algae at concentrations of ] and 2 PPM. The
algae were left in contact for one hour, one day and ten
days. The: protocol for these tests involved procedures
described in the Water and Waste Water Manual of the
United States Public Health Service. The exposure tests
involved post inoculation in order to determine
whether the devices were algicidal or algistatic. The
oxidizing agent for activation was sodium persulfate at
a concentration of 10 PPM. The devices were found to
be algistatic at 1 PPM and algicidal at 2 PPM after one
hour’s exposure. After one day and ten days, there were
no positive flasks at all. Ten flasks of subculture were
utilized for each test, and only one flask was positive out
of ten after one hour at 1 PPM.

While there is shown and described herein certain
specific examples embodying the invention, it will be
manifest to those skilled in the art that various modifica-
tions and rearrangements of &he invention may be
made without departing from the spirit and scope of the
underlying inventive concept and that the same is not
limited to the particular forms herein shown and de-
scribed except insofar as indicated by the scope of the
appended claims.

What is claimed is:

1. A method for killing pathogens including bacteria,
viruses and algae in utilitarian water bodies including
the water of swimming pools, industrial cooling towers,
hot tubs and drinking supply reservoirs, which com-
prises adding to the water a multitude of tetrasilver
tetroxide molecular crystals which are capable of elec-
trocuting said pathogens via an electron transfer mecha-
nism involving their molecular structure in the presence
of oxidizing agents.

2. A method as claimed in claim 1 where the oxidiz-
ing agent is a persulfate.

3. A method as claimed in claim 1 where the concen-
tration of the molecular crystals in the water is a maxi-
mum of one part per million.

4. A method as claimed in claim 2 where the concen-
tration of the molecular crystals in the water is a maxi-

mum of one part per million.
se ee *