'1'.» TKlfg-IJ 1"" " ‘ "
flair-1.13 l; A ‘.’f' ., v

1"” J ”7.5".“
:‘11243. v

[‘1 (J

 

THE. DETERMINATION OF 10010.83

1N STABKLIZED 'xODiZED SALT

Thesis for the {Degree of M. 5.
MiCHIGAN STATE COLLEGE
Laura Huntley Anderson

1944

‘h‘:Un:(on9.l‘o-o.~:iy.o.¢......

ram)

T h

THE DETERMINATION OF IODIDB IN

'STABmZED IODIZID SALT

by

Laura Huntley Anderson
-M

A'IHESIS

Suhnitted to the Graduate School of Michigan
State College of Agriculture and Applied
Science in partial fulfilment of the
requirements for the degree of

MASTER OF SCIEQCE

Department of Bacteriology

Year 1944

The Deteminati on of Iodides in Stabilized Iodized Salt*
INTRODUCTION

The abnormally high parentage of persons affected with goiter in
the state of Michigan has long been a public health problem of considerable
simificence. The incidmce of goiter in Michigan prior to the use of
iodine supplmants was probably higher than that in any other region of
the world, with the exception of Switzerland. This incidmce was emphasized
by the selective service registration of 1918 which showed that goiter
was so prevalent in some groups, in northern Michigan and Wisconsin that
as hid: as 3) per cent of the persons exmnined were incapacitated for army
service, owing to disqualifying toxic goiters (1). This widespread pre-
valence of goiter had been a matter of common knowledge for years and was
accepted by the populace as an environmental malaw for which there was
no relief. No serious consideration had been given the situation by the
state medical profession until 1921 when the first stimulus for an active
miter cunpaign was occasioned by Levin's paper, reporting that of 1,783
persons in Lake Linden, Michigan, 1,146 had thyroid enlargeth (2). This
observation was immediately followed by a Michigan Department of Health
survey in J'anuary, 1922, of residents of Iron Mountain, Michigan. This
survey revealed that 54 per cent of the persons examined had perceptible
mlarguents of the thyroid (3). In another survey by Reed and Clay of
Grand Rapids, Michigan, so per cent of the school children examined were

found to have enlargement of the thyroid gland (4). The publication of

* This study was conductedat the Bureau of Laboratories, Michigan Depart-
maIt of Health, Lansing, Michigan, financed in part by a grant from the
Salt Producers Association through their chumittee on Simplified
Practice and Standardization.

160531

2.

these data clearly pointed out the need for a public health program for
the prophylaxis of simple goiter in Michigan.

While it is now almost universally agreed that iodine deficiency is
the cause of simple goiter, there has been a great deal of discussion as
to the methods of supplying iodine for the purpose of prophylaxis.
Refermces to the popular folk ranedy of the time of giving burnt cork as
a remedy for witer and cretinian date back as far as 1280 A.D. Iodine
was discovered by Courtois in 1811, and isolated from the sponge by Byte
in 1819. In 183) Coindet, a physician in Geneva where goiter was prevalent,
postulated that iodine was the goiter-curative principle in burnt sponge
and further obtained dranatic results using the new element for treating
conditions of iodine deficiency. However, indiscriminate use of the new
elenart produced toxic effects and it was not until the present century
that iodine prophylaxis and therapy were accepted as sound medical and
nutritional practice.

The first large scale experiment in goiter prevention was begun in
this country in 1917 by Marine and Kimball in Akron, Ohio, where a survey
of grade and high school girls revealed a goiter incidence of 56 per cmt.
Approximately one-half of the 4495 children examined were each given, in
0.2 an doses distributed over a period of tvo weeks, a total of 2 an of
sodiun iodide in drinking water, and the other half were given no iodine.
This procedure was repeated twice a year and provided mough iodine to
saturate the thyroid. At the end of four years all the children were
reemined. Of those who were nomal when the adninistration was started,
and took iodine as directed, none developed goiter, while of those who
did not take iodine, 27.6 per cmt developed goiter. Of those who had

goiters and who took iodine systenatically, the thyroid gland returned to

5.

nomel size in more than 60 per cent of the cases, while of those who
did not take iodine, only in comparatively few did the thyroid gland Show
any tendency to decrease in size (5, 6, 7, 8, 9, 10).

Following Kimball's first publication in 1917, Klinger in inrich,
Switzerland, in 1918, began iodine therapy in the school children of that
city, since it previously had been feund that in some of these schools
100 per cent of the children were goiterous. Instead of the sodium iodide
used by Marine and Kimball, Klinger used iodostarine chocolate tablets
which were an iodized fatty acid (tariric acid diiodide) combined With
chocolate and made into tablets, each containing 5 milligrams of iodine.
This was a.non-hygroscopic, stable preparation, and a farwmore pleasant
medicant than sodium iodide. This method was employed in three cantons
in Switzerland with even more striking results than those obtained by
Marine and Kimball in this country. In one canton the goiter incidence
was reduced.from.87.6 per cent to 13.1 per cent in feur years (10, 11).
Thus the value of iodine prophylaxis has been unquestionably established
for twenty-five years but further proof of its usefulness has been established
by more recent investigations.

The most notable recent investigations are the extensive studies
made "in Michigan and Ohio. In 1923 and 1924 the Michigan State Departnent
of Health conducted a survey in various sections of the state to determine
the correlation between the incidence of goiter in school children, and
the amount of iodine in the water supply. The feur counties of.Macomb,
Midland, Hexford, and Houghton were selected as showing the greatest

variations in iodine content of the ground waters and as being representative

4.

of a cross section of the population of Michigan. The iodine content
of the ground waters in these four counties varied from 0 to 8.7 parts per
billion. ‘me total number of children examined in the four counties was
65,537 of whom 38.6 per cent had goiter. The incidence of goiter in each
of these four regions was inversely preportional to the iodine content
of the water. In the county having the highest iodine contentvof the water
apply, the incidence of goiter was only 26 per out, as contrasted to.
64.4 per cent in the area having no iodine in its ground water (12).
Imediately following this survey a state-wide campaign was begun
by the Michigan State Department of Health to cnphasize the fundamental
causes of endemic goiter and the principles of its prevention. In the
spring of 1924 a special committee was appointed by the Michigan State
Medical Society to work with the State Department of Health on this
problen. These two groups, representing the medical profession of the
state, cooperated with the Wholesale Grocers' Association and the Salt
Ianufacturers' Association with the result that beginning May 1,1924,
the salt manufacturers produced and put on the market throughout Michigan
an iodized salt containing one part of potassium iodide to 5,000 parts
of salt (0.02%). There was no law compelling people to use the iodized
salt but the wholesale grocers did all they could to promote the sale
of only this salt, and the State Department of Health carried on an active
cunpaign to educate the public to its use. The program carried on by
these groups included an estimation of goiter incidence during the ten-
year period from 1924 to 1934, as indicated by records of goiter operations,
and a re-survey of goiter incidence in school children.
In 1928, four years after the introduction of iodized salt, 50,134

of the school children exmined in the 1923-24 survey were rs-examined and

5.

the incidmce of goiter was found to have dmpped from 38.6 per cult to

9.9 per out. At the and of the ten-year period a final survey showed a

further radiation to 8.2 per cent throughout Michigan. Among those using

iodized salt during the entire ten-year study the incidence of goiter

was only 2.88 per cent (13). The results of the entire ten-year study

are best summarized by Dr. R. D. McClure, Chief Surgeon of Henry Ford

Hospital, and a member of the State Medical Society Committee on 31nd

Goiter (14).

1. Iodized salt as used in Michigan did at first apparently increase
the number of thyroid operations.

2. The increase was in the nodular goiter or adenoma group, and we believe
the iodized salt may have activated a group of quiescent adsnomata,
producing toxic goiter symptans.

3. The increase reached its peak in the second year after the introduction
of iodized salt. '

4. An increase in the death rate from goiter as shown by the Board of
Health statistics reached its peak in the second year after the intro-
ducticn of iodized salt.

5. There was no increase in hyperthyroidism, excepting in the nodular
goiter or adenomata group.

6. The number of operations for toxic, diffuse and toxic nodular goiter
has rapidly and steadily decreased after the apex of the second year
in crease had been reached. .

7. The incidence of endenic goiter or enlarged thyroid has been reduced
almost to nil since iodized salt has been so widely used.

8. We now see no cases which show the slightest ill effects from the use

or iodi zed salt.

6.

9. Toxic nodular goiter and toxic diffuse goiter are less apt to occur
whal there has been no previous enlargenent of the thyroid (endenic
goiter); at least this would seen a safe conclusion based on experience.

In 1936 Kimball made a survey in the Cleveland, Ohio, parochial
schools to detennine the effect of the use of iodized salt on the incidence
of goiter. Of those using iodized salt 7 per cent were affected with
goiter as compared with 30.7 per cent of those not using it. The incidence
of goiter in the latter group had been found to be essentially the same in
a survey 12 years'earlier (13).

The foregoing studies present ample evidence that iodized salt is
effective as a prophylactic measure for goiter. In this connection McCollum
stated Moreover, there are other aspects of health than t h e prevention
of goiter. Hypothyroidism or conditions of hyperplastic activity, owing
to iodine deficiency, are accompanied by defects other than deformity of
the neck. Mental development, sexual maturation, and the development of
positive persenality are retarded. Hence, iodine supplementation, insofar
as it corrects or prevents a goiterous condition, promotes these functions,
and contributes to the maintenance of good health." (15).

The excellent results obtained in the 1924-35 survey in Michigan
stimulated an interest among public health leaders to allow other states
to share the benefits of Michigan's experience through the services of a
national organization. Consequently, a Study Committee on Eidenic Goiter
was organized in and under the direction of the American Public Health
Association. This committee, together with the Michigan State Medical
Society's Committee on Iodized Salt, and the National Research Council,

Camuittee on Food and Nutrition, presented the following resolution

'7.

which was adopted by the Michigan Medical Society Committ es in May 1940,
and by the American Public Health Association Committee in June 1941.

"Resolved, That all salt for table use of human beings and the salt
used for feeding to domestic animals in the United States should contain
one hundredth of one per cent of Potassium Iodide or its equivalent viz.,
forty-five milligrams of Potassium Iodide to each pound of salt, provided
that an effective stabilizer be used.”

The lowering of the level of potassium iodide flom the two hundredths
per cult previously used was made possible by the incorporation of a suitable
stabilizer for the potassium iodide. An effective stabilizer for the
potassium iodide content of iodized salt had been formulated through
work at the University of Wisconsin resulting in the issuance of a patmt
to the Wisconsin Alumni Research Foundation (16). In non-stabilized
iodized salt losses as high as 100 per cent of the potassium iodide were
not uncamnon. These losses are due to the formation of hydriotic acid and
the subsequent liberation of elemental iodine and are accelerated by
storage under warm, moist conditions or the presence of slight impurities in
the salt such as traces of copper, iron, or manganese salts. Acid salts
such as magnesium chloride or calcium chloride also will act on the
potassimn iodide producing hydriotic acid. To counteract the formation of
hydriotic acid, alkaline salts such as magnesium carbonate, sodium bicarbon—
ate, calcium phosphate, and cal cium oxide are now enployed as stabilizers.
The oxidation of hydriotic acid to elemental iodine is prevented by the
use of reducing agents such as sodium thiosulfate or dextrose. These
alkaline salts and reducing agents are used in various mnbinations in
camercial stabilizers depmding to some extent on tin natural impurities

present in the salt.

8.

The decreased iodine content of iodized salt and the use of various
reducing agents as stabilizers made questionable the reliability of exist-
ing methods for the determination of anall quantities of iodine in salts.
Therefore, this study was initiated to evaluate analytical procedures for
the determination of iodides in stabilized iodized salt for the purpose of
selecting methods which could be made official by the Association of
Official Agricultural Chanists and would be acceptable to the Federal Food
and Drug Administration.

In October, 1945, the author was made Associate Referee on Iodides
and Bromides for the Association of Official Agricultural Chemists, re-
placing Major J'. T. Tripp, Michigan Department of Health, who had pre-
viously held the position.

The appointment of the A.O.A.C. Associate Referee on Iodides and Bromides
to the American Public Health Association Committee on Standard Methods
prevented duplication of work. Further coordination was secured by the
appointment of members of the American Medical Association and National
Research Council Committees to the American Public Health Association
Cmittee on Bhdanic Goiter. Manbers of the salt producing industry were
invited to present the technical difficulties incident to the newly adopted
reduction in potassitml iodide content and to suggest the technical needs
of the industry regarding control methods.) The salt producing industries
cooperated by offering the services of their analysts as collaborators
and by supplying salt samples and details of manufacture.

The work to date has been divided into two phases. Phase I was a
collaborative study designed to evaluate the methods routinely used by

control analysts in the laboratories of seventeen collaborating salt

9.

producers. Each analyst was asked to use a method of his own choice in
analyzing the smiples suhnitted to him. Phase II also was a collaborative
study designed to evaluate further tuo methods which gave satisfactory
remlts and which were most frequently selected by the collaborators in
Phase I of the study. Each analyst was asked to use the two specific methods

in analyzing the samples submitted to him in the second phase of the study.

INVESTIGATION
PHASE I. Comparison of results obtained with methods selected and used
by commercial analysts.
Source of samgles; companies and locations.

Nine salt producing canpanies located in various areas throughout
the United States and anploying different stabilizers collected 24 cartons
of iodized salt at random from their production lines.
wrench of samples.

Code numbers frail 1 to 9 were assigied to the salt samples from the
nine differalt producers. These nine salt samples were prepared as
follows for distribution to seventeen collaborating analysts: The contents
of ten of the cartons from each company were pooled and thoroughly mixed.
Aliquots of the salt were accurately weighed, and 20 liters of a 20 per
out solution were prepared from each of the nine salt samples submitted.
Sufficient acid (concmtrated H2804 or concmtrated 1101, depending on the
(nature of the stabilizers) was added to dissolve the stabilizers. The

Quantities of acids were as follows:

10.

 

 

 

Sample No. Stabilizers Acid added per liter solution
1 MgOOg, 0.75 ml conc. H2804
2 Mg003 0.50 " " "
3 Mgmg 1.00 " ' "
4 083(P04)2

NaHOOs 0.89 " " H01
Dextrose
5 M3005 0.75 " " H2804
6 Ca3(P04)2 2.00 " " HCl
7 M8003
Nazszos
8 C83(P04)2 2.00 " " HC].
1‘18ng
9 Ca3(PO4)2 2.76 " " "
NaHCOs

The solutions were dispensed in amber glass bottles, sealed with .

'Celoseal" caps, and labeled to show sample number, concentration of salt,

and kind and amount of acid added.

 

Collaborating analysts.
Aliquots of all nine samples were submitted to each of seventeen

collaborating analysts who was asked to use a method of his choice in

analyzing each sample for per cent iodine.

Methods employed.

Seven different methods of analysis were selected by the collaborating

‘ analysts.
I.
V II.

III .

The methods anployed are listed below.
Elmslie-Caldwell (l7)
Sadusk-Ball (18)

Potassium cyanide.
Original reference not available.

11.
IV. Tentative method for Waters, Brine and Salt, Association of
Official Agricultural Chemists (19).
V. Woodward (20).
VI. Fresenius (21).

VII. Modified Viebock and Breckner (22, 23).
Modified by New York Station of Food and Drug Administration.

Results and conclusions.

The results submitted by the seventeen collaborating analysts are
presmted in Table l. The suthor is coded as analyst L.

The two most popular methods as evidenced by the number of analysts
who_selected than were the Elmslie-Caldwell (17) (Method I, Table l) and
the Sadnsk-Ball (18) (Method II, Table 1) methods. Both procedures gave
satisfactory results as judged by their distribution about the mean values.
The other five methods (Methods III, IV, V, VI, and VII, Table l) were
less frequently used and while the results in some cases were apparently
erroneous there are not data sufficient to prove or disprove their value
as analytical procedures. By the same token there were not data sufficient
to Justify the acceptance of either Method I or Method II as completely
satisfactory procedures. These data only indicate that Method I and Method
II were employed most frequently by this collaborating group of analysts
and that the resultsobtained showed deviations that were within reasonable

limits.

PHASE II. Comparison of Elmslie-Caldwell and Sadusk-Ball methods.
Source of samples: Companies and location.

Four salt producing companies located in various areas and anploying
differalt stabilizers collected cartons of iodized salt from their pro-

duction lines at specified time intervals during two consecutive days.

12.

Eggparation of samples.

The salt samples were prepared as follows for distribution to the
twelve collaborating analysts: Code letters A, B, C, and D were assigned
to the salt samples from.the four different producers. To each of the
code letters was added the sample number given by the individual producers
denoting order of collection (e.g., A91, Ar2, A23, etc.). Each sample
was prepared by pooling and thoroughly mixing the contents of four cartons
bearing the same code letter and number (e.g., Arl). Aliquots of salt
were accurately weighed, and 6 liters of a 20 per cent solution prepared
frmm each of the samples collected at specified.intervals by the four
campanies. One ml of concmtrated H2804 per liter of solution was added
to each sample to dissolve the stabilizers. The solutions were dispensed
in amber glass bottles, sealed with ”Colossal” caps, and labeled to show
sample.nmmber, concentration of salt, and amount of’HESO4 added.
Collaborating‘gnalysts.

Six collaborating analysts were sent samples A—l to A-9 and B—1 to
3-9, and six analysts were sent samples 0-1 to 0-9 and D-l to D-6. However
one analyst failed to su'umit results, and another analyst experienced tech-
nical difficulties and was unable to submit an acceptable report. It was
unfortunate that both analysts had received the C and D series of samples.
Methods employed.

The collaborating analysts were naked to analyze the samples for per
' cart iodine by both the Elmslie-Caldwell (l7) and Sadusk-Ball (18) pro-
cedures, which in Phase I of the study gave satisfactary results, and were

most frequently selected by the collaborators. The procedures are as follows:

H
()3
0

Method I. Elmslie—Caldwell (1?)
Reagents

(a) Sodium thiosulfate solution.-- 0.005 N. Dissolve 12.4 g of reagent-
grade Na28203.5H20 in freshly distilled H20 and dilute to 1 liter
giving an approximately 0.05 N stock solution. Prepare 0.005 N
solutions by dilution of this stock solution with freshly distilled H20.

(b) Standard Potassium Iodide solution.“ Prepare a solution containing
exactly 0.1308 g of reagent-grade KI (0.1000 g 12) per 1 liter of
freshly distilled H20.

Reactions

 

2M: + 63r2+ 6H20 - 21(103 + 12 HBr

K103 + SCI + 2H3P04 - (file + 2K3P04 + 5H20

2Na28203 + lg - Na28406 + 2NaI
Determination

The following method of analysis is the Kinslie-Caldwell method with
the imition step omitted.

Take 25 m1 aliquots of the so per cent salt solution, add 5 g of -
Na2005, cover with watch-glass and boil gently for 10 min. Transfer contents
to 18 cm filter paper and wash with boiling H20, catching filtrate and
washings in 500 ml Erlenmeyer flask (solution should total ca 500 ml).
Neutralize to methyl orange with 85% 1131304, and add 1 ml in excess.

Add excess of Br water and boil solution gently until colorless, and
then 5 min. longer. Add a few crystals of salicylic acid and cool to
ca 20°. Add 1 m1 of 85% 1131904 and ca 0.5 g of KI and titrate I with
0.005 N Na28203 in the usual way, using starch solution as indicator.

Standardize the NagSgOg solution by measlring into a 500 ml Erlenmeyer

exactly 25 ml of the standard solution containing 0.1338 g of XI per liter,

l4.

adding 300 m1 of H20 and 5 g of N82003, neutralizing, and proceeding as

directed above. (It is advisable to standardize the Na28203 solution same

day deteminations are conducted).

Method II. Sadusk-Ball ( 18) .

(a)

(b)

.(c)

(d)

(6)

Reagents
Sulfuric acid.-- 2 N. 1 volume of concentrated £12804 plus 1'7 volumes

of freshly distilled H20.
Bromine vapor.-- Blow air (washed with H20 and dried by C8012)
through a gas washing tube containing 0. P. bromine. Deliver vapors
just above the liquid in the flask.
Potassium iodide solution.—- 10%. Prepare a KI solution containing
10 g reagent-grade KI per 100 m1 (freshly prepared).
Sodimn thiosulfate solution.-- 0.005 N. Dissolve 1.24 g of reageit-
grade Na28203.51-120 and 3.8 g crystallized borax (Na2B4O7.10H20) in
freshly distilled H20 and dilute to 1 liter. The solution is standard-
ized immediately before use by titration gainst standard K103
solution.
Standard potassium iodate solution» 0.005 N. Prepare a stock solution
containing exactly 3.567 g reagmt-grade KIOgiper liter, giving a 0.1 N
solution. The stock solution is further diluted to give a 0.005 N
reagent.
Reactions

2KI+ 6Br2+ 6H20= £103+12HBr

K103 + m + 552304 = 312 + 5320 4» 5K2804

2 N828203 + 12 = NagS405 + 2 N81

Deteminati on

 

Transfer a 5 g portion of the salt and lOO ml of freshly distilled

'- H20 to a 200 ml Erlenmeyer flask and mix the contents of the vessel until

l4.

adding 500 m1 of H20 and 5 g of Na2005, neutralizing, and proceeding as

directed above. (It is advisable to standardize the M25203 solution same

day deteiminations are conducted).

Method II. Sadusk-Ball (18).

Reagents

(a) Sulfuric acid.-- 2 N. 1 volume of concentrated 112804 plus 17 volumes
of freshly distilled H20.

(b) Bromine vapor.-- Blow air (washed with HBO and dried by CaClg)
through a gas washing tube containing 0. P. bromine. Deliver vapors
just above the liquid in the flask.

‘ (c) Potassium iodide solution.-- 10%. Prepare a K1 solution containing
10 g reagent-grade KI per 100 ml (freshly prepared).

(d) Sodium thiosulfate solution.-—- 0.005 N. Dissolve 1.24 g of reagent-
grade Na28205. 5H20 and 3.8 g crystallized borax (Na2B407.10H20) in
freshly distilled H20 and dilute to 1 liter. The solution is standard-
ized immediately before use by titration against standard K103
solution.

(6) Standard potassium iodate solutionc- 0.005 N. Prepare a stock solution
containing exactly 3.567 g reagent-grade KInger liter, giving a 0.1 N
solution. The stock solution is further diluted to give a 0.005 N
reagent.

Reactions
2K1+ 6Br2+ 611302 $103+12HBr
K103 + SKI + 3112804 = 312 + 3120 + 5 K2804
2 N828203 + I2 ' NagS406 + 2 N81

Determinati on

 

Transfer a 5 g portion of the salt and 100 ml of freshly distilled

_ '1 H20 to a 200 m1 Erlenmeyer flask and mix the contents of the vessel until

solution of the sodium chloride has taken place. Add methyl orange
indicator and introduce 2. N H2304 drop by drop until a pink color results
which persists on standing. After the addition of 2 ml of 31112804 and
Br vapor, add a few glaSs beads and boil the solution until the yellow
color due to bromine disappears and then for 2 minutes longer. Upon
cooling, wash down the sides of the flask with approximately the amount
of water lost by boiling. Add 2 ml of a 10% K1 solution (freshly pre-
pared), gently swirl the contents of the flask, and titrate liberated
iodine imediately with 0.005 N thiosulfate, adding 2 m1 of starch indicator
near the end point.
Resultsand conclusions.

The results of the twelve collaborating analysts are given in Table 2.
The author is coded as analyst 6. These data show that with one exception,
there was close agreement between the results submitted by individual
analysts, and that the Elmslie-Caldwell and Sadusk-Ball methods are equally
suitable as analytical procedures for the determination of iodine in
stabilized iodized salt. These data have been subjected to graphic and
variance analyses which confirmed these conclusions.
Recovery eQeriment s.

In order to evaluate further the two methods for the determination
of iodine in stabilized iodized salt, recovery experiments were performed.
In both procedures reagent-grade K103 (Bakers analyzed) was used to stand-
ardize the 0.005 N Na28203 solution. The iodine contents of the iodized
salt solution and of the stock KI solution were determined by a series of

6 analyses on each, and mean values were used in the calculation of the

16.

recoveries. The results of these recovery series are given in Table 3.
These data are in agreement with those previously presented, and further
indicate that both methods are sufficiently accurate for the determination
of iodine in stabilized iodized salt.

Summary_and recommendations made to the Committee on Waters, Brine and

 

Salt; Association of Official Agricultural Chemists.

In a collaborative study it was found that the Klmslie-Caldwell and
Sadusk-Ball methods of analysis for the determination of iodine in stabilized
iodized salt were most frequently employed for routine analyses in the
laboratories of salt producers. The results of the collaborative study
and the recovery experiments performed show that both methods are sufficiently
accurate and reproducible for the purpose designated.

0n the basis of these findings, the author as Associate Referee on
Iodides and Bromides, A.0.A.C. presented the Referee for Waters, Brine, and
Salt with the following recommendations:

1. That the Elmslie-Caldwell method be considered for adoption as

an official method for the determination of iodides in stabilized
iodized salt.

2. That the Sadusk-Ball method be considered for adoption as a
tentative method for the determination of iodides in stabilized
iodized salt.

As a result of these recanmendations the Association of Official

V Agricultural Chemists has adOpted the Elmslie-Caldwell method as official
(first action) for the determination of iodine in salt (24). Official
action on the Sadusk-Ball method has been deferred pending further

collaborative work (25)” s.

Collaborating Analysts
Organi zation

American Salt Company, Kansas City,
Missouri

Barton Salt Company, Hutchinson,
Kansas

Carey Salt Company, Hutchinson
Kansas

*Colonial Salt Company, Akron, Ohio

*Diemond Crystal Salt Company, St. Clair,
Michigan

*Hardy (Manistee) Salt Company, Manistee,
Michigan

*International Salt Company, Watkins
Glen, N. Y.

Jefferson Island-Salt Company,
Jefferson Island, La.

Leslie Salt Company, Neward, California

Michigan Department of Health,
Lansing, Mich.

*Morton Salt Company, Chicago, Ill.
Myles Salt Company, Weeks, Louisiana
*Ohio Salt Company, Rittman, Ohio
*Union Salt nonpeny, Cleveland, Ohio

U.S. Department of Agriculture,
Washington, D. C.

*Watkins Salt Company, Watkins Glen, N. Y.

Wisconsin Department of Agriculture,
Madimn, W180

*Woroester Salt Company, Silver Springs,
New York

17.

shim
Kansas City Testing Laboratory

R. S. Humphreys

L. A. Enberg

L. 0. Judy

H. W. Diamond
F. G. Miller
J. E. LaPorte

C. G. Lindstrom

A. Marciniak

J‘ . Gran t—Mackay

D. S. See

Laura Huntley

C. H. Martin

Staff chemists

T. R. Rader

The Textor Laboratories

R. A. Osborn

E. Le‘dense

F. D. Everett

* Salt companies supplying samples of cannercial iodized salt for the study

 

18.

A_cjcnowledgnents
The author wishes to express her appreciation to all collaborating
analysts and salt producing companies, to Mr. W. G. Wilcox, Chaiman,
Committee on Simplified Practice and Standardization, Salt Producers
Association, to Major J. T. Tripp, Associate Referee at the time this study
was begun, and to Dr. H. C. Batson for his direction and suggestions on

this study.

 

1.

2.

3.

4.

5.

6.

8.

9.

10.

11.

12.

13.

14.

15.

16.

1'7.

19 .
BIBLIOGRAPHY

Levin, Simon, Goiters in Five Hundred and Eighty-three Registrants,
.T. Mich. State Med. Soc. 18, 98 (1919).

Levin, Simon, One Thousand One Hundred and Forty-six Goiters in One
Thousand Sevm Hundred and Eighty-three Persons, Arch. Int. Med.,
31, 421, (1921). ’

Olin, R. M., Iodine Deficiency and Prevalence of Simple Goiter in
Michigan, I. Am. Med. Assn., 83, No. 17, 1328 (1924).

Reed, Torrance, and Clay, H. T., A Survey of Thyroid Enlargement
Among the School Children of Grand Rapids, Pub. Health Man., Mich.
Dept. of Health, _l_l_, 287 (1923)

Marine, David and Kimball, O. P., The Prevention of Simple Goiter,
J. Lab. 8c Clin. Med., _3_, 40 (1917).

Marine, David, and Kimball, 0. P., The Prevention of Simple Goiter
in Man, Arch. Int. Med., _2_2_, 41 (1918).

Marine, David, and Kimball, 0. P., Prevention of Simple Goiter in Man,
J’. A. M. A., 13, 1873 (1919).

Marine, David, and Kimball, 0. P., Prevention of Simple Goiter,
Arch. Int. Med., _2_5_, 661 (1920).

Marine, David, and Kimball, O. P., Prevention of Simple Goiter,
J'. A. M. A., 11, 1068 (1921). '

Kimball, O. P., The Prevention of Simple Goiter in Man, Am. J. Pub.
Health, 1g, 81 (1923).

Klinger, R., Pmphylaxis of Eldanic Goiter, Wien. klin. Wchnschr, _3_§,
35 (1922); abstr. J". A. M. A., Z_8_, 1175 (1922).

Eldridge, E. F., The Iodine content of the Water Supplies of Michigan,
Am. J'. Pub. Health, }_4_, No. 9, 750 (1924).

Kimball, 0. P., Prevention of Goiter in Michigan and Ohio, I. A. M. A.,
108, 860 (1937).

McClure, R. D., Thyroid Surgery as Affected by Generalized Use of
Iodized Salt in Ehdanic Goiter Region- Preventive Surgery. Ann. Surg.,
100, 924 (1934).

McCollum, E. V., Ormt-Keiles, Elsa, and Day, H. G., The Newer Knowledge
of Nutrition, the McMillan 00., Ed. 5, 254 (1939).

U. 3. Patent No. 2,144,150, Jan. 17, 1939.

Methods of Analysis, A.O.A.C., 58, p. 368 (1940).

18.

19.

22.

23.

24.

25.

20.

Sadu‘sk, :r. F., and Ball, E. G., Volumetric Determination of shell
Quantities of Inorganic Iodine, Ind. Eng. Chem, Anal. Ed., §_, 386 (1933).

Methods of Analysis, A. O. A. C., 102, p. 547 (1940).

Woodward, M. IL, Iodized Salt as a Convenient Method of Administering
Iodine to Animals, Mich. Dept. of Ag. Bull., _:_3_a_, 11, (1924—5). Cited by
Geagley, W. C. (1929) in Snell, Colorimetric Methods of Analysis,

1, 569 (1936).

Funnan, N. H., Scott's Standard Methods of Chanical Analysis, Ed. 5,
l, 454 (1939).

Viebock and Breckner, Pham. incnats" 19, 191 (1929).

Clark, E. P., Smimicm Determination of Halogens in Organic Compounds,
I. A. O. A0 Co, 2.1, 486 (1934).

I. A. 00 A. Co. g, No. 1, 11° (1944).

LIA. o. A. C., 31, No. 1, '71 (1944).

 

 

-——1

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

‘38. _ 88. 88. 88. 3.8., 88 ....o .1
080. $8. 88. some. 38. 8.8. .58. 8%.
agile
88. m 08¢. a
88. o 3.8. H
due. 2 88. e 88. u
38. 5 e80. .— 88. a some. 0 38. o
mono. $8. 38. m 88. a «mac. n 88. m 88. e
lflaw o. 3.4le e o ammo. . a Bdojaguu
£8. 38. 88. 88. 38. 2.8. 3.8. 5:.
jg o (no
88. m 2.8. a
2.8. o 38. H
. . Did» p or. I... «G H goat U glare)
88 88 2.8 m 2.8. a 88. a 2.8. m 2.8.
Nana. o. a a4 30. gel. No.31)
$0 .38 38. 88. :8. 88. 88. rum
3.8. a
88. a 88. a
88. m 88. n
m m
5 3.2.45 an 3322
, _._.>i§jz lllldaflulieu a

 

ecuoao sec .32.» «c 3.930. surname-I .3575. «53:30:00 an vasugoev no end-I weave.

 

 

 

 

:04ICAHC«

 

mono. oono.lkooo. «0.8.

an «M. NH.
3.5%. I .5: - ,

H 3003 H .nvefl H :30: ,

nouns... we.” ee- .3 84 £89. an... .8 888 ufleteee. .. code: I. 8 Ta 88...
88.... .86 one a. 88.8 28738 2. 3a.»: .1. 8 n4 :88

 

 

 

 

 

 

  

 

 

 

 

. 68.3.3 «0 305.! «Hamil—Gum 35 e8 805801385 .3. e5
.3534. 3:18 undo-honed"... F «05503 no :1- 0383 .3 «i=3 a

u GAO-u.

 

 

 

 

 

 

 

 

      

   
   

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

* Obviously erroneous, not include

 

I
. B. Samples C-l to 1
) Samples D—l to 1
_A_naly§t 7 vAn'avly ‘1
Time of Math. I teeth. °n
collection
Met!
9% I --
i“ £12811. day .0065 .0058 ,3,
.0062 .00
First day .0054 .0055 .===‘
0-2 10 a.m.
_fi » .0054 .00
t ' First day .0044 .0045
‘ 0-3 12 noon
1 ' _;9944 .00
f’ _ First day .0036 .0056
’0-4 2 p.m.
. A .0054 .00
f’ Second day .0065 .0061
.0-5. 9-a.m. ‘
.0065 .0
. Second day .0079 .007
C-5. 10 a.m.
; . .0080 .0 """
fr“ : Second day .0065 .005
{(3-7 12 noon
_, .0065 .0<
F” 2 Second day .0057 .0054
(0-8- 1 p.m.
L11 .0056 .0 -——-
7’ Second day .0062 .005 ry
'. C-9 2 p.m.
. r .0065 .0 ____
" First day .0070 .006 ""
11:50 a.m.
.0069 A41
First day .0087 .008
1 p.m.
.0086 .0
First day .0074 .007
1:30 p.m.
.0075 .0
First day .0071 .006
am p.m.
\ .0071 ..
First day .0083 .006
3:30 p.m.
.0085 .5 ""’
First day .0076 .001
4 p.m.
.0075 J

Recoveries of iodine added as KI to 25 m1 of a 20% iodized salt solution

Table 3

 

 

 

   

 
   

 

 

 

 

 

 

 

 
 
     

 

A. By the Elmslie-Caldwell method
I content
Trial 0 iodized 12 added 1 Determined Recovery
number salt solution 12
mgs 7 mgs mgs "mgs %
1 .6714 .2236 .8950 .8979 100.32
2 " .2236 .8950 .8817 98.51
3 n O 4472 1 6 1186 1. 1122 99 043
4 " .4472 1.1186 1.1214 100.25
5 “ .8943 1.5657 1.5948 101.86
6 fl .8943 1.5657 1.5927 101.72
B. By the Sadusk-Ball method
12 content
Trial of iodized 12 added Determined Recovery
number salt solution IQ '

ommet-I

 

fl

 
 

mgs mgs mgs

.2236 .9209 .9194
.2236 .9209 .9206
.4472 1.1445 1.1468
.4472 1.1445 1.1427
.8943 1.5916 Lost

.8943 1.5916 1.5974

 

 

 

 

99.34
99.97
100.21

99.85

100.36

 

 

 

{‘5 (“3’1“ USE ONLY

.5915

‘w‘

1'.

(Ii

6”:

 

 

“TIT ififlfli'ufiliflujn fififlflfiflifi 111113111111”