chemical investigations of

Project Report NO. 39 ('.

DFO - Library I MPO - Bibliotheque

11111111111111111111111111111111111111111111111111

C da Fisheries SeNice. Industrial ana . cr REPORT

Development Service. PROlE

99939229

CHEMICAL INVESTIGATIONS OF

Chondrus crlspus

by

James A. Rigney, Ph.D., Department of Chemistry.

University of Prince Edward Island. Charlottetown, P.E.I.

(Progress Report, 1970)

for

Industrial Development Branch, Fisheries Service,

Department of Fisheries and Forestry, Ottawa

May 1971

Chemical Investigations of Chondrus crlspus

(Progress Report, 1970)

by

James A. Rigney, Ph.D., Department of Chemistry,

University of Prince Edward Island, Charlottetown, P.E.1.

This was a project carried out for the Industrial Development Branch, Fisheries Service, Department of Fisheries

and Forestry, Ottawa May 1971

•

...

TABLE OF CONTENTS

Summary ............................................................. . Page 2

Introduction ....................................... . ................ . Page 3

Analytical Procedures ............................................... .

Plant Age and Chemical Analyses ..... , ............................... . Page 6

Effects of Storage Conditions on Chondrus Crispus ................... . Page 8

Miscellaneous Fractions of Carrageenan ............ '" ............... . Page 11

Relocation of Routine Analytical Work ..... '.' ....................... . Page 14

Samples from Areas Other than Miminegash, Prince Edward Island ...... . Page 14

Program Proposals Page 15

APPENDIX I PROCEDURES

I

II.

III.

IV.

V.

Preliminary Treatment of Samples .... '" .............. Page 16

Extraction of Carrageenan "" """"" .......... '" ........ Page 16

Fractionation of Carrageen an . " .. '" . """ " "",." . "" . " """ Page 17

Determination of Viscosity .. ." .... " "" ",,"",,"""" """ """" " Page 18

Determination of Gel Strength " "" ".,,"" ,,"",,"" " ". " """""" Page 19

APPENDIX II - ANALYSES OF CHONDRUS CRISPUS

Table of Carrageenan Analyses Page 20

Table of Additional Analyses ......................... Page 23

The program dealing with Chondrus crispus on which this report

is based is a continuation of one drawn up by the Department of Fisheries

and Forestry, Marine Plants Experimental Station at Miminegash, Prince

Edward Island, and the author in the spring of 1968. The primary object

ive was the increased knowledge of this important marine plant, commonly

called Irish Moss, from which is extracted carrageenan, a widely used in

dustrial and food additive.

During the first summer of the project the main accomplishment

was the design of analytical procedures which would allow the monitoring

of various chemical constituents and properties of Chondrus crispus. The

following summer of 1969 was spent mainly in using the analytical proce

dures on various samples of Chondrus crispus most of which were from the

Miminegash area in attempts to establish correlations between various pa

rameters of seasons, properties and components.

This report summarizes the work of the third year, 1970, in

which emphasis was placed on the age of the plant as a strong influence

on other parameters, and on the further study of promising indications

from the previous year's investigation. Recommended studies for 1971

are also included.

The author would like to acknowledge with gratitude the coop

eration of the staff of the Marine Plants Experimental Station, and es

pecially Mr. Claude Wallace and Mr. Donald Jones. In addition to Mr.

Jones, Messrs. Glenn Wood and James Gairns of the University of Prince

- 2 -

Edward Island were also involved in the design and performing of these many

analyses.

Summary

1) Approximately five dozen samples of Chondrus crispus were ana-

lyzed for their carrageenan contents according to the procedures described

last year. Many of the extracts so obtained were also analyzed further as

to their components and properties. While most of the samples were from

Prince Edward Island, at least a dozen samples were obtained from other

maritime provinces.

2) Data from samples culled as to age of component plants, have

given firm indications that meaningful correlations are now possible. On

the other hand, data from samples which were picked with no allowance for

the age of the component plants continue to support little or no correla

tions.

3) Storage techniques developed last year were studied further.

Dry storage in bales led to no obvious change in properties since May,

1969. Wet storage in various strengths of lime water does not adversely

effect properties either although the very encouraging results of last

year regarding pure white products, high yields and a high Kappa/Lambda

ratio were not substantiated in the present work.

4) The routine analytical work has been successfully relocated

from the University of Prince Edward Island to the Marine Plants Experi-

- 3 -

mental Station at Miminegash. This move will increase efficiency of the op

eration because of the proximity of the analytical work to the main sample

points and because of the greater possibility of work continuing on a yearly

basis rather than just during May - September which has been the practice.

S) Miscellaneous studies including the instrumental analysis of

carrageenan (unsuccessful) and additional fractionation of Kappa carrageenan

(successful) have been pursued.

Introduction

Chondrus crispus, or Irish Moss as it is commonly known, is the

red marine plant used most widely as the source of carrageenan, an important

commercial product in industrial and food additives. The chemical structure

of carrageenan is somewhat similar to that of cellulose, both being polymers

of sugars or saccharides. One important difference between these two natu

rally occurring polysaccharides is that the sugar units in cellulose are of

glucose while in carrageenan they are of galactose. Another important dif

ference is that while there are no acidic groups attached to the polymers in

cellulose, the carrageenan polysaccharide contains almost one sulfate mono

ester group per sugar unit. The acidic characteristic of carrageenan caused

by the high sulfate content accounts for many of its important properties, e.g.

its ability to form hydrocolloids or gels in water.

The properties of carrageenan also depend on the proportions of its

- 4 -

two main fractions, Kappa and Lambda. The fractions differ in their amounts

of sulfate (Lambda having more) and the fact that the Kappa fraction contains

an inner oxygen bridge, called an anhydro linkage, on alternating sugar units.

The different structures of the fractions lead to different properties. For

example, the Lambda fraction is considered responsible for higher viscosity

while the Kappa fraction imparts greater gel strength in the presence of

potassium ions.

The paucity of information on the relationship between the vari

ous chemical characteristics and properties of the carrageenans prom~ted

this study.

Analytical Procedures

During 1969 as many as fourteen tests were run on some samples in

attempts to obtain worthwhile correlations between properties and between

properties and seasons. Because of the lack of success in establishing cor

relations, emphasis this year was placed on the more routine inspections as

% total carrageenan and its viscosity, % Kappa fraction and its gel strength,

and % Lambda fraction and its viscosity. The procedures for these inspections

are reported in Appendix I and are essentially as reported last year. How

ever a few comments should be made.

Tests on the precision of the analytical procedures continue to

be very encouraging. While fewer such tests were run this year, data from

samples 21, 23 and 38 show an average difference between duplicate runs of

- 5 -

0.8% total carrageenan. Comparisons with sample 38 and with samples last

year, on the other hand, indicate a 3.4% average discrepancy between du

plicate determinations of Lambda and Kappa contents. This is not complete

ly acceptable especially for the interpretations that will be called for

in the future. It is hoped that precision here will be improved.

While the patent literature cites the use of ethyl alcohol as

a precipitating agent for carrageenan, present indications are that lower

yields, especially of the Kappa fraction, will result from using this sol

vent. Having experimented with this alternate solvent, all future precipi

tations will rely on the more common isopropyl alcohol technique.

In attempts to streamline procedures, the ether washings of the

Lambda fraction were omitted only to find that a hard, light tan carragee

nan resulted. The softer, whiter product obtained after ether treatment is

preferable.

- 6 -

Plant Age and Chemical Analyses

The almost complete lack of any correlations in the analytical

data last year strongly suggested that possible seasonal variations were

being confused by the presence in each sample of plants of different ages

in varying concentrations. Because differences in chemical properties among

the plants might very well exist, some emphasis was placed on the plant age

effect. Three times during the season rather complete analyses were run of

four different age catagories in each sample. The age classification which

was employed was that of Dr. A. R. A. Taylor of the University of New Bruns

wick who has assigned seven stages to the growth of the Chondrus crispus

plant. Because of few plants being present in some distinct age groups,

group pairing was done. The results are summarized in Table I.

The data give good indication that:

1) The younger plants (Groups 1 - 4) undergo the greater changes

during a season, increasing either their total carrageenan content or their

Kappa/Lambda ratio.

2) The oldest plants (Group 7) underwent little or no change in

their composition and properties over the test period. All inspection ex

cept one viscosity value are remarkably similar for this group.

3) The older a plant, the greater the Kappa fraction, with this gen

erality extending to the increased age of the young plants over a single

season. In addition, the gel strength of the Kappa fractions generally tend

TABLE I

Season Effects on Age GrouQs

6/4/70 8/4/70 10/4/70 , . \

Groups T A K V'J VA GK K/).. T A K VT v).. G

K KIA T A K VT v).. GK t<A

1 & 2 26.3 50.9 20.2 63.5 0.40 54.2 43.1 30.2 233 310 161.5 0.69

I 0.63 43.7 17.8 64.0 320 3.60 41.3 22.1 57.1 443 185.7 2.58

I j

3 & 4 43.6.151. 6 35.3 •

,

5 % 6 58.0 30.0 53.2 86.0 1. 78 35.0 28.8 53.1 1.85 43.9 18.5 63.7 963 264.5 3.32

7 54.0 24.4 57.0 2.34 50.0 26.5 58.9 253 2.22 53.5 24.0 61.0 530 990 195.6 2.55 , ~

,. I T , = % total carrageenan

A = % Lambda fraction

K = % Kappa fraction

VT = Viscosity of total carrageenan in cps.

VA = Viscosity of the Lambda fraction in cps.

GK = Gel strength of the Kappa fraction in grams, Bloom

- 8 -

to increase over the season. The seasonal increase of the Kappa fraction,

apparently at the expense of the Lambda compound, has been discussed pre

viously.

4) Considering mainly the 10/4/70 series of samples, there appears

to be good correlation between the viscosity of the Lambda fraction and

age of the plant, and at least some correlation between the Kappa fraction

content, the gel strength of the Kappa fraction and the age of the plant.

The direct applicability of plant age effects to harvesting or

to processing is not as great as the above indications may appear. Harvest

ing the Chondrus crispus by raking actually takes much more of the older

plants than the younger ones because of the bushier profile that Groups 5,

6 and 7 offer to the rake. However, some younger plants do become entrained,

and because of their changing composition may be effecting analyses and even

commercial yields in a manner which inhibits correlations and forecasts.

It should be mentioned that analyses were run on extra samples

from just Groups 5, 6 and 7 during June and July, 1970 and that their results

tend to detract from the above conclusions. Just such lack of agreement de

mands that complete analytical data be obtained on all age groups at least

once a month over an extended period of time. The indications here for in

creasing our knowledge of Chondrus crispus are definitely promising and

should be pursued further.

Effects of Storage Conditions on Chondrus Crispus

In a continuation of the experiment begun last year the effects

- 9 -

of two different storage techniques were investigated. One technique used

storage in bale form in the atmosphere within the Marine Plants Experimental

Station at Miminegash, Prince Edward Island. The other technique was in

vOlved with storage in seawater containing various concentrations of lime.

The material which had originally been mechanically dried and

baled in May, 1969 had shown no significant change during the remainder of

that year, as reported last yea!. The same bale was analyzed three times

during 1970 and indicated that a slight change may have occurred. This in

dication, if it is real, was manifested mainly in the total carrageenan and

its Lambda fraction. The following table summarizes the data from 1969 and

1970.

Date

5/27/69

6/27/69

7/30/69

10/22/69

6/15/70

9/ 4/70

10/16/70

Core Samples from Dried Plant

(baled 5/69)

% Total Carrageenan

48.3

53.6

50.4

53.8

47.8

41.7

44.6

Viscosity (cps)

77

62

71

235

91

88

- 10 -

As suggested last year some differences from sample to sample are

probably to be expected because of the heterogeneity of the bale itself as to

the age of the component plants. This may explain the apparent 6.8% average

decrease in total carrageenan. However another inspection, the viscosity of

the total carrageenan, seems to have maintained its original value. Because

of doubt in the case of change in the 1969 bale and no ind~cation of change

in the case of the 1970 bale (samples 13, 36, 48), this storage technique

will be investigated further over the next year to observe the significance

of the data.

Last year several samples stored in water were analyzed and gave

some encouraging indication of the possible benefits of wet storage. One

of the most encouraging techniques was the use of seawater containing 4%

lime. The one sample that was stored in this medium for almost three months

was most unusual for its high yield, low viscosity, pure white products and

high Kappa/Lambda ratio. This interesting lead was therefore studied in

1970 to check reproductibility of these results and also the effects of sev

eral levels of lime. The pertinent samples are 50, 51, 52. In a sense, the

more recent results are disappointing. None of the benefits which were ten

tatively assigned to lime water reoccurred. In fact, the Kappa fraction was

even a little darker than is normal with untreated samples. However, no ad

verse effects were noticed and the level of lime between land 4% in the

storage water seems to be immaterial.

In this study the limewater storage technique was checked only

- 11 -

over the first two months. The experiment having been set in operation will

continue in order to find the effects of time.

Miscellaneous Fractions of Carrageenan

The two major fractions of carrageenan are Kappa and Lambda. The

differences between these two fractions described in the introduction, would

imply that there are distinct boundaries of properties between them. However,

it is known that there is a continuum of variable structural forms which has

the true Kappa form as one limit and the true Lambda form as the other. In

such a scheme there is no consideration of molecular weight differences be

tween the various polymer chains. Further, there has been little consider

ation of molecular weights in general as they might relate to the properties

of carrageenans. This interesting relationship was a posed as a consequence

of the continuing evaluation of our analytical techniques. In both instances

cited below an additional type was isolated which gave indications of being

somewhat differe~t from the usually isolated Kappa and Lambda fractions.

In the first instance, the solutions of isopropyl alcohol and

water which remained after the removal of the total carrageenan product,

would yield additional product after being cooled. At times, only an unre

coverable haze would result but with some samples agglomerates of material

would form which, when isolated and dried, would approach significant am

ounts, e.g. 1% from sample 25, and 3.01% from sample 10. Because of the

small absolute amounts which were isolated, no tests were run on these frac

tions.

- 12 -

In the second instance, ethanOl which was used to wash the Kappa

fractions to remove water also dissolved a type of carrageenan which resem

bled the Kappa fraction from which it came. This new material, called the

Omega fraction just for designation here, amounted to 3.4% of the total

carrageenan of sample 7 and a very high 16.4% of sample 6.

The following table compares its properties with those of the

other fractions of sample 6.

,fomparisons of Fractions from Sample 6

Fractions % Sulfate Gel Strength,

Lambda 50.9 26.2

Kappa 20.2 14.1 63.5 ~~

Omega 16.4 15.0 nil

These points should be considered:

gm.

1) Part of the very common discrepancies between (%K + %)J and 10~/o

may b~ due to Omega material.

2) The resemblance of the Omega material to the Kappa fraction is

stronger than to the Lambda fraction.

3) The removal of the Omega material with its lower gel strength

benefits the remaining Kappa fraction. Kappa carrageenan may

therefore be upgraded by ethyl alcohol washing.

* When run on the refrigerated gel, the strength was 37.7 gm.

- 13 -

4) The high amounts of this ethyl alcohol soluble material in this

particular sample (# 6) may be a consequence of the young age

of the plants in it (Groups 1 & 2).

In each of the examples of additional carrageenan types being

obtained, the effect of solubility, while it could be .due to increases in

polarity of the polymer, much more strongly suggests the presence of lower

molecular weight materials. Indeed, separations of different molecular

weight fractions of polymers are often realized by reliance on the decreas

ing solubilities of the larger molecules in mixed solvents of a series of

concentrations.

Instrumental Analyses of Carrageenans

Because of the differing environments of the protons in the Kappa

and in the Lambda fractions, a study was made of the use of nuclear magnetic

resonance as a tool to analyze total carrageenan for its two main fractions.

This technique uses a modern spectrometer, recently obtained by the Univer

sity of Prince Edward Islad, which is extremely sensitive to just such dif

ferences as exist in the Kappa and Lambda fractions. However, rather con

centrated solutions of samples which are quite fluid are required. This

combination of solution properties could not be obtained in the two deut

erated solvents in which carrageenans are soluble, water and dimethylsul

foxide. The study was therefore abandoned.

- 14 -

Relocation of Routine Analytical Work

Almost all of the work described in the reports of the last three

years has been performed at the University of Prince Edward Island in Char

lottetown, Prince Edward Island. While it was proper to do the early work,

as the design of analytical procedures and equipment. in the setting of the

University's Biochemistry Laboratory, efficiency and also Convenience is

better served by relocating the routine operations to the Marine Plants Ex

perimental Station at Miminegash into which port most of the seaweed samples

arrive. Thus besides better coordination between sample gathering and

analysis, the possibility of year-round operation will be a definite advan

tage. The recent acquisition of an Atomic Absorption Analyzer at the Mimi

negash Station will also permit additional worthwhile analyses to be run

there. Studies of a less routine nature will continue to be performed at

the University where research equipment and instruments are available.

Eamples from Areas Othen than Miminegash

Fourteen samples of Chondrus crispus from areas other than Mimi

negash, Prince Edward Island, were received and analyzed. Two of these were

from other areas of Prince Edward Island while twelve were from the rest of

the Maritimes. The results from these samples gathered with no consideration

of the ages of component plants really serves only as a service to interested

parties. However, just such a service may disclose unusual results which

could be indicative of a situation which should be examined further. One

- l~ -

definite indication from the present work is that there is little difference

between machine drying and ground drying on the % total carrageenan (see sam

p les 21 & 22).

Program Proposals

The following topics are recommended for study in 1971.

1) complete analytical date on the plants of different ages as they

progress throughout a year. Samples should be at most one month

apart;

2) continuation of the storage experiments with possible consider

ation to the effect of the container on the color of the carra

geenan products;

3) isolation of sufficient amounts of the additional types of carra

geenan so that these materials may be characterized;

4) the application of other analytical techniques to the understand

ing of the carrageenan structure. Electrophoreses will be con

sidered.

The rationale for each recommendation is contained in this report.

Submitted by

- 16 -

APPENDIX I

PROCEDURES

I. Preliminary Treatment of Samples

The plant samples were usually received after having been oven

dried. However, to insure against the bacterial decomposition which can

occur in moisture, and also to obtain a base weight, the samples were

dried when received at 600

C. overnight. After chopping and sifting to

remove sand and obvious impurities, 60 grams of the sample was further

dried at 400

C. overnight in a vacuum oven.

II. Extraction of Carrageenan

Twenty grams of dried Chondrus crispus was digested in 1900 mI.

distilled water for two hours at 900 C. (The upper limit for this treat

ment was 930C.) The resulting mixture was strained through a wire gauze

(14 - 40 mesh) to yield a filtrate which was centrifuged at 6000 - 7000

r.p.m. in a Servall S5 - 4 centrifuge. The clear centrate was collected,

and the residues from straining and centrifuving were re-digested in 1000

mI. distilled water at 900 C. for two hours. The straining and centri

fuging were repeated and all clear centrates were combined.

The combined centrates were slowly mixed with twice the volume

of isopropyl alcohol (99%) while stirring vigorously. (Best isolations

were achieved when the carrageenan solutions were fresh and warm, i.e.,

- l"'l -

while at 40 - 500

C., and soon after centrifuging the second digestions.)

Difficulties were encountered when the isolation was conducted on day-old

solutions, although an inert atmosphere was found to retard degradation

here. Unless the carrageenan was of a high Kappa fraction content, the

fibers of the isolated product clung to the stirring mechanism and could

be easily scraped off. Centrifuging was useful when some product remain-

ed suspended in the water-alcohol mixture.

The carrageenan product was separated from excess liquid by

centrifuging, the solid was washed in 500 mI. of ethanol and then in

300 mI. of ethyl ether before being filtered through a Buchner funnel

(no vacuum, no filter paper). The filtrate was recycled through the

funnel until it was clear. After air drying in the funnel over the fil

trate, the product was v.acuum dried at 400

C. overnight. The percent

yield based on the dried plant was then calculated.

III. Fractionation of Carrageenan

Into 2100 mI. of distilled water was dissolved 7.00 grams of

carrageenan using a stirrer and moderate heat. After cooling to room

temperature, a solution of 41.7 grams of KCI in 700 mI. distilled

water was added while stirring. The resulting soft gel was centrifuged ~~

(Servall SS - 4, at 7000 - 8000 r.p.m.) . The residue and the centrate

,;, Difficulties in obtaining a completely dry product were experienced when centrifuge speeds of less than 5000 - 6000 r.p.m. were tried.

- 18 -

were both saved.

The residue was washed in a homogenizer in 2 x 280 ml. ethanol,

separating the phases after each washing by centrifugation. The washed

residue was then treated with 300 mI. ethyl ether in the homogenizer and

filtered through a Buchner funnel containing filter paper. The residue,

which was the Kappa fraction of carrageenan, was dried in a vacuum oven,

wieghed and its percent yield calculated.

To twice its volume of isopropyl alcohol was added, with stir

ring, the centrate from the original KCl induced separation. The pre

cipitate, which was the Lambda fraction of carrageenan was ~ither col

lected manually on a stirrer or by centrifugation, and was then washed

in ethanol and ether as was the Kappa fraction above. After drying in a

vacuum oven, the Lambda fraction was weighed and its percent yield cal

culated.

The ethanol washings of the Kappa fraction were mixed with

twice the volume of isopropyl alcohol and the resulting gelatinous pre

cipitate collected by centrifugation. This products was washed in ethanol

ethyl ether (1:1) then ethyl ether and finally dried of all vapor. For

lack of a better term, this fraction of carrageenan was called "Omega".

IV. Determination of Viscosity of Carrageenan Solutions

Into 350 mI. of distilled water was dissolved, by boiling, 1.75

grams carrageenan (either total or fraction). The solution was cooled to

- 19 -

250 C. and the weight adjusted back to 350 grams by adding distilled water. o

The viscosity was then measured at 25 C. on a Brookfield Viscometer, model

LVF, using the # 1 spindle and 60 r.p.m.

V. Determination of Gel Strength of Carrageenan Solutions

Into 175 mI. of distilled water was dissolved, by boiling, 2.52

grams of carrageenan in a tared 400 mI. beaker. When the solid was dissolved,

or after 1 1/2 hours, 25 mI. of water containing 0.48 gram KCI was added,

and heating and stirring continued. When solution had occurred the weight

was adjusted back to 200 grams and poured in a dish, 70 mm. wide, 50 mm.

high, so that the surface of the gel was 1/4" above the edge of the dish

(tape was attached around the edge). After refrigeration overnight, the

tape was removed, and after the gel warmed to room temperature its gel

strength was measured on a Bloom Gelometer.

- 20 -

APPENDIX II

Table I

Carrageenan Analyses of Chondrus Crispus

::( Date % Total Sample #- Description 1970 Carrageenan

1 Fogo Island , Newfoundland 2/ 49.9

2 Skinner's Pond, P. E. 1. 5/12 52.5

3 Group 7 5/14 50.8

4 Raked 5/15 49.6

5 Group 7, St. Peters, P. E. 1. 5/18 51.3

6 Groups 1 & 2 6/4 26.3

7 Groups 3 & 4 6/4 43.6

8 Groups 5& 6 6/4 58.0

9 Group 7 6/4 54.0

10 Combined Groups 6/4 37.0

11 Group 7 6/15 48.1

12 Dry Storage ( 1969 ) 6/15 47.8

13 Dry Storage (1970) 6/15 44.3

14 Groups 5 & 6 6/15 36.5


* All samples with no designation of origin were harvested at Miminegash, Prince Edward Island.

- 21 -

Date % Total Sample # Description 1970 Carrageenan

16 Blue Cove, New BrunswicJ( Spring 44.5

17 Pubnico, Nova Scotia 7/3 41.6

18 Groups 5 & 6 7/3 37.5

19 Group 7 7/3 34.4


21 Machined dried 7/8 41.1 Pubnico, Nova Scotia 40.2

22 Ground dried 7/8 40.6 Pubnico, Nova Scotia

23 Combined Groups 7/18 41.2 41. I

24 Groups 5 & 6 7/18 48. I

25 Group 7 7/18 35.0

26 Neguac, New Brunswick 7/19 26.0

27 Poin t Sa pin, New Brunswick 7/20 39.6

28 Blue Cove, New Brunswick Summer 33.6

29 Groups 3 & 4 8/4 43.7

30 Groups 5 & 6 8/4 35.0

31 Group 7 8/4 50.0



34 Polly's Cove, Nova Scotia 9/3 48.2

- 22 -

Date % Total Sample "# Description 1970 Carr ageen an

35 Dry Storage ( 1969) 9/4 41.7

36 Dry Storage ( 1970) 9/4 41.1


38 Test Sample 9/24 43.7 42.2

39 Combined Groups 9/'213 52.2

40 Ketch Harbour, Nova Scotia 10/1 59.7

41 Groups 1 & 2 10/4 54.2

42 Groups 3 & 4 10/4 41.3

43 Groups 5 & 6 10/4 43.9

44 Group 7 10/4 53.5


46 Fresh water washed before 10/5 50.9 drying

47 Dry Storage ( 1969) 10/16 44.6

48 Dry Storage ( 1970) 10/16 42.5

49 Stephenville, Newfoundland 10/21 55.5

50 1 % Lime water storage 11/27 41.5



53 Blue Cove, New Brunswick 12/21 40.9

APPENDIX II

Table II

Analyses of Chondrus Crispus

Table of Additional Analyses

Total Lambda Kappa

II II II Sample Date % Viscos. % Viscos. % II II 1J: Description (1) 1970

II ( 2) cps. I ( 3) cps.

II ( 3)

I I

II II II II II

II I! 1 Fogo Island, Newfoundland 2/ II 49.9 67.5 12.8 69.7

II II 2 Skinner's Pond, P. E. 1. 5/12 II 52.5 II

50.5 82.7 31.0 II II

5/14 " II 46.6 II

41.6 3 Group 7 II 50.8 51.3 II II 1/ II II

5/15 I 49.6 45.8 300 II

4 Raked II

II I I

5 Group 7, St. Peter's, 5/18 51.3 I 41.0 37.3 I 1/ P. E. 1. I I II

II II II 6 Groups 1 & 2 6/4 26.3 II 50.9 II 20.2

II II

7 Groups 3 & 4 6/4 43.6 II 51.6 II

35.3 II

1/

1) all samples with no designation of origin were harvested at Miminegash, Prince Edward Island. 2) % carrageenan of dried plant. 3) % of total carrageenan 4) grams, Bloom

Ge 1 (4) Strength

202

68.2

178

115

63.5

II II II I

II Ii I

II " II II II

II II

II II II

II

~

5.43

0.63

0.89

0.91

0 .. 40

0.68

N W

Total Lambda Kappa

Sample Date II 0/ Viscos. I % Viscos. I % Ge I (4) II /0 II II Ii # Des cr i pt ion (1) 1970

II ( 2) cps. II ( 3) cps. II

(3) Strength ,

Ii Ii

Ii II Ii II

II II II II

11 Ii I

Ii I I

Groups 5 & 6 6/4 58.0 30.0 I

53.2 86.0 1. 78 8

II " I

II I I

6/4 54.0 II 24.4 I

57.0 II

2.34 9 Group 7

II II Ii II II

II 10 Combined Groups 6/4

"

37.0 50.5 II 36.8 0.73

II /I

16 Blue Cove, New Brunswick spring I 44.5 44.6 II 45.6 181 1.02 I I I Ii II

18 Groups 5 & 6 7/3 I

37.5 461 I

II II II II

23 Combined Groups 7/18 II 41.2 168

II II 41.1 II

II r I

26 Neguac, New Brunswick 7/19 I 26.0 121 I I I I I I

11

I

28 Blue Cove, New Brunswick I 33.6 37.0 34.6 157 I 0.94 summer I I I

II

II I

29 Groups 3 & 4 8/4 II 43.7 17 .8 64.0 319.3 II

3.60 II

/I II

30 Groups 5 & 6 8/4 II 35.0 II 28.8 69.0 I 53.1 II 1.85 /I II II II II

31 Group 7 8/4 II 50.0 26.5 II 58.9 II

2.22 II 253 II II

II II I

32 Combined Groups 8/15 II

51. 2 275 I II I II

II I

I II

33 Combined Groups 8/31 50.2 259 II

II II I II II I II

II /I I II 34 Polly's Cove, Nova Scotia 9/3 II

48.2 35.4 II 48.0 126 II II II 1.36 II II II

, .

Total Lambda Kappa

Date II

% Viscos.

If % Viscos. II % Gel (4) 11

Sample

"

I Description (1) 1970 ( 2) ( 3) (3) Strength I

# cps. cps. II

I II

I II I I II II I I

I! I II I I

II I

Dry Storage ( 1969) 9/4 /I 41.7 90.6 I

36.2 181 48.8 1.35 35 I I I I I /I 36 ( 1970) 9/4

I 41.1 32.0 I 37.0 56.6 46.4 132 Dry Storage I I /I 1. 25 I I I I II

37 Combined Groups 9/14 I 45.0 303 I 1/ I I

II

I II 38 Test Sample 9/24 43.7 I 37.8 55.6 104 1.47 I I /I 42.2 I 42.0 I 53.3 III 1.27

/I I /I II I 39 Combined Groups 9/28

II 52.2 88.0 I

II II II I II II I 40 Ketch Harbour, Nova Scotia 10/1

II 59.7 Ii 36.3

/I 47.7 119 " /I II 1. 32 I /I Ii 41 Groups 1 & 2 10/4 54.2 232.5 I 43.8 310 30.2 162 0.69 I /I I II I

II II

42 Groups 3 & 4 10/4 41.3 I 22.1 443 57.1 186 II

2.58 I II I

II /I

43 Groups 5 & 6 10/4 43.9 I 18.5 963 61.7 264 II 3.32 II

II

II II

44 Group 7 10/4 II

53.5 530 II 24.0 990 61.0 196 /I 2.55 II II II II I II /I 45 Combined Groups 10/4

" 44.0 320 I /I II I

II II

46 Fresh water washed before 10/5 \I 50.9 I 39.2 42.9 178 /I 1.09 I II II drying I II

II I /I II I II

II II II II

II 47 Dry Storage ( 1969) 10/16 II 44.6 87.9

" II

" II \I II

40 Dry Storage ( 1970) 10/16 /I

42.5 31.4 106 II

49.2 II

1.57 /1 II II

II II II

Total Lambda Kappa II II II II Sallllple Date /I % Viscos. II % Viscos. % Ge 1 (4) /I II

1t Des cript ion (1) 1970 II (2 ) cps. (3 ) cps. II (3) Strength II II II II Ii

II II II

II Ii III Ii

II

II !I !I II II I II II

II I I II 49 Stephenville, Newfoundland 10/21 55.5 I 13.3 I 63.6 4.79 II I I II I I

II II I I 50 1% Lime Water Storage 11/27 II 41.5 I ;}3 .8 53.9 177 1.;}3 II I II II II

I 51 2% Lime Water Storage 11/27 46.3 II ;}3.7

II 54.0 II 1. 39

II !! II

r .. . ,

chemical investigations of

Documents