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T ECHNICAL A PPLICATION I NFORMATION Herbstreith-Pektinometer Mark IV

TECHNICAL APPLICATION INFORMATION

T ECHNICAL A PPLICATION I NFORMATION Herbstreith-Pektinometer Mark IV

Herbstreith-Pektinometer Mark IV

I NTRODUCTION The Herbstreith Pektinometer Mark IV is a fur- ther development of the Herbstreith

INTRODUCTION

The Herbstreith Pektinometer Mark IV is a fur- ther development of the Herbstreith Pektino- meter Mark III which has already been estab- lished since more than fifteen years. It is used for the determination of breaking strength of gels, especially of pectin gels which are pro- duced with high and low methylester pectins.

In the following we would like to introduce to you the device as well as some typical examples for application for the reasonable use of this device in quality control and product develop- ment.

The method for determining the firmness of the gel by measuring the breaking strength has been developed as a modern method from an ancient, oftentimes proved procedure which was already published in 1927 by Luers and Lochmüller. With this method the inner breaking strength of a pectin gel is evaluated according to the tensile loading necessary to pull a central shear insert out of the gel and with that to disrupt the gel.

The first and very simple measuring device was the Pektinometer from Luers consisting of a balance. Here the shear insert was pulled out of the gel by weighing the scale down with shots. Soon the balance was replaced by an arrestable spring balance which was connected with an electric motor. In further development steps the spring balance was replaced by an electronic force measuring system which finally resulted in the development of the Herbstreith Pektinometer Mark II in 1983.

Finally in 1988 the Herbstreith Pektinometer Mark III was developed, a measuring device controlled by a micro controller.

Meanwhile the Herbstreith Pektinometer is widespread and used successfully for an objec- tive determination of the gelling behaviour of pectin gels in quality control as well as for product development.

Above all the request for an extended measur- ing range, for a timely and modern data re- cording and for a user-friendly and pleasing design finally lead to the development of the Herbstreith Pektinometer Mark IV.

to the development of the Herbstreith Pektinometer Mark IV. 2 H ERBSTREITH & F OX Corporate

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HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de

Using the Herbstreith Pektinometer Mark IV the breaking strength (inner firmness) of a pectin gel is assessed regarding which tensile loading (force) is necessary to pull a standar- dised shear insert out of a standardised meas- uring beaker being filled with a defined gel in order to disrupt the gel.

During pulling out the shear insert at constant velocity the force is measured by a strain gauge continuously over a defined time period. From the curve progression the maximum force in HPE is determined. This value is a measure for the inner firmness, i.e. the breaking strength of the gel.

Constant measuring conditions during the dis- rupting procedure are the precondition for reproduceable results. They are assured at the

Herbstreith Pektinometer Mark IV by the follow- ing allegations:

• controlled rotation speed of the motor by a rotational-speed sensor

• controlled measuring time

• taring of the force recording (tara) before each measurement

• standardised measuring beakers and shear inserts

The progression of the force-time-curve addi- tionally gives information concerning the con- sistency (texture) of the gels. Therefore the Herbstreith Pektinometer Mark IV records the force progression during the disrupting proce- dure and assesses it. From the quotient of maximum force (HPE) and integral of the force-time-curve the so- called texture constant K is determined with which a conclusion concerning the gel’s tex- ture becomes possible.

concerning the gel’s tex- ture becomes possible. Elastic brittle, i.e. little spreadable gels break at a

Elastic brittle, i.e. little spreadable gels break at a relatively high force input. Afterwards the shear insert slides through the broken gel for which only a minor force input is necessary as the broken gel does not resist the shear insert to a great extent. The force-time-diagram shows relatively high and narrow peaks, the values for the texture constant K are comparably high.

the values for the texture constant K are comparably high. Fig. 1: Force-time-diagram of an elastic-brittle

Fig. 1: Force-time-diagram of an elastic-brittle gel

Elastic viscous, i.e. very smooth and spread- able gels do not break that simple. The shear insert is pulled through the gel under a steady force input as the gel resists the shear insert during the whole measuring procedure. The force-time-diagram shows wide peaks with flank, the values for the texture constant K are comparably low.

the values for the texture constant K are comparably low. 3 Fig. 2: Force-time-diagram of an

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Fig. 2: Force-time-diagram of an elastic-viscous gel

HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de

E QUIPMENT CONFIGURATION and technical data Equipment configuration The Herbstreith Pektinometer Mark IV consists of

EQUIPMENT CONFIGURATION

and technical data

Equipment configuration

The Herbstreith Pektinometer Mark IV consists of the following modules:

• 2 motherboards

• NETDCU with software

• gear motor

• DMS measuring stirrup uptake and force measuring amplifier

• LCD display with touch panel

• thermo printer

• ethernet connector

Key control elements of the Herbstreith Pektin- ometer Mark IV are the user-friendly LCD dis- play with touch panel which among date, time and sample number also shows breaking strength (HPE), integral of force-time-diagram, the texture constant K calculated herefrom and force-time-diagram.

By means of a thermo printer additionally all relevant data are printed.

If necessary after measurement the measuring results can be processed by a pc or network server connected to the ethernet. For this pur- pose the Herbstreith Pektinometer Mark IV re- cords each final 500 files.

Technical data Measuring value uptake: DMS measuring stirrup uptak with amplifier

Measuring range:

Measuring exactness:

20 g – 3000 g ± 1% from measuring value, < 5 HPE 10 mm/s 60 mm 30 mm

Speed of extension:

Distance of extension:

Measuring distance:

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HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de

C OMPARISON OF Herbstreith-Pektinometer Mark III and Mark IV The determination of the breaking strength

COMPARISON OF

Herbstreith-Pektinometer

Mark III and Mark IV The determination of the breaking strength with the Herbstreith Pektinometer Mark III is a method which has been widespread since many years. Therefore the new Herbstreith Pektino- meter Mark IV has been conceived that way that it provides values comparable to the for- mer model at simultaneously improved meas- uring technique.

This responds to the demand that the results

of both devices can be directly compared to

each other which is especially in the range of

quality control and product development of great importance.

A new property of the Herbstreith Pektinome-

ter Mark IV is the measuring range which has been extended from 50 – 2000 HPE to now 20 – 3000 HPE. With that also very firm gels can be measured now.

Additionally the Herbstreith Pektinometer Mark

IV offers the possibility to characterize the tex-

ture of the gels, i.e. the elastic resp. elastic vis- cous properties by means of the texture con- stant K which is issued with each measuring protocol.

Furthermore the Herbstreith Pektinometer Mark

IV possesses an internal memory which is con-

ceived for recording each final 500 files.

With that the user has the possibility to process the measuring values by pc connected to the ethernet resp. to record them digitally.

The handling for adjustment resp. calibration of speed and force of extension of the device has been essentially simplified for the Herbstreith Pektinometer Mark IV.

The extension speed of 10 mm/s is controlled by the gear motor also under load and does not have to be checked or adjusted.

Also the extension force is already calibrated from the producer for the whole measuring range so that an after-adjustment is no more necessary. A control of the extension force e.g. within control of inspection, measuring and test equipment can be done with suitable stan- dardised weights. Then the thermo printer prints a check protocol stating the measured value as well as the mass of the used stan- dardised weight.

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HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de

T YPICAL Applications Typical applications for the reasonable use of the Herbstreith-Pektinometers Mark IV in

TYPICAL

Applications

Typical applications for the reasonable use of the Herbstreith-Pektinometers Mark IV in quality control and product development.

For the standardization of high and low methyl- ester pectins traditionally the so-called ridge- limeter method is used. This method describes the production of a pec- tin-sugar-acid gel (65% ss, pH 2.2) under defined conditions. After 24h the stableness under its own weight is measured (Cox and Higby, 1944). From this method the standardisation to gelling strength in °USA-Sag was developed which is relevant for pectins and widespread as trading basis for pectins (IFT, 1959).

This internationally accepted method disting- uishes itself primarily by its simple handling and good reproducibility.

Disadvantages for the pectin users are mainly the unpracticable recipe parameters such as low pH-value of the product and the missing buffer substances from the fruit. A further criterion also is the relatively long standing time of 24h which is necessary before starting the meas- urement and obtaining results.

As gels being produced according to the ridge- limeter method are not becoming destroyed during the measuring this method basically detects elastic properties which do not always

correlate with the real inner firmness, i.e. brea- king strength.

In contrast to that the pectin gels are charged up to the destruction of the gel network when determining the breaking strength with the Herbstreith Pektinometer. The force necessary for this effect is measured.

As jams and jellies are also destroyed while spreading, chewing and swallowing or when taking them out of the packaging, the breaking strength determined with the Herbstreith Pek- tinometer corresponds to the impression of the consumer which is noticed as sensoric gel strength.

For determination of the gel strength by means of breaking strength with the Herbstreith Pek- tinometer Mark IV almost user-defined recipes (model gels, gel preparations close-to-practice e.g. jellies, jams) can be used. With that it is possible for the user to assess gels which are exactly tuned towards his requirements. For reproducible measurement it solely is ne- cessary that the produced gel preparations gel and that fruit components – if they are used – are grinded fine resp. show a relatively small particle size and are distributed homogeneously.

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HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de

When using a suitable recipe it is therefore pos-

sible to characterize high methylester, low me-

thylester and high resp. low methylester, ami-

dated pectins by the determination of breaking

strength over a relatively wide ss and pH range.

Furtheron by suitable recipe selection the results

of the breaking strength determination by using

the Herbstreith Pektinometer Mark IV can be al-

ready obtained after very short standing time

of the gel (e.g. after 2h).

after very short standing time of the gel (e.g. after 2h). a) Standard model for assessment

a) Standard model for assessment of high and

medium methylester pectins (e.g. incoming

goods inspection for pectins)

For a quick and reproducible assessment of pec-

tins in the field of incoming goods inspection or

quality control often standard model gels are

prepared. Depending on the recipe the breaking

strength can be determined already after a

standing time of 2h.

In such model gels the fruit part of a gel prepa-

ration is replaced by a suitable buffer solution.

As especially in the field of quality control re-

With that it is possible to exclude quality vari-

producible results are quickly requested and in

ations caused by the fruits.

the field of product development the assurance

The obtained breaking strength correlates with

of sensoric impressions by means of objective

the firmness which the pectins will reach in

measurements is required, the determination

jams and jellies.

of the breaking strength with the Herbstreith

Pektinometer Mark IV is a reasonable and nec-

Recipe parameters

essary supplementation to the ridgelimeter

Soluble solids content: 65%

method.

pH-value in final product: 3.10 ± 0.05

This is demonstrated with three typical appli-

cations in the following.

Buffer solution: Potassium acetate / lactic acid

buffer solution

Pectin dosage: 0.100% – 0.275%

The determination of breaking strength is done

at 20° C, 2h after preparation of the gel.

strength is done at 20° C, 2h after preparation of the gel. 7 Fig. 3: Breaking

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Fig. 3: Breaking strength of a standard model gel in dependence from pectin dosage citrus pectin DE° 58%, 150° USA-Sag (65% ss, product pH-value 3.1, potassium acetate / lactic acid buffer solution, pectin dosage 0.100% - 0.275%)

HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de

b) Standard model gel for assessment of low

methylester amidated pectin (e.g. production

control for household gelling sugar)

For production control of household gelling

agents sugar-acid gels are often prepared with

water or buffer solutions. For preparation of the

gels a complete compound consisting of e.g.

sugar, pectin and buffer substances can be used.

The breaking strength which often can be

determined after a relatively short standing

time (e.g. after 2h) provides information on

quality and homogeneity of the investigated

gelling sugar batch.

and homogeneity of the investigated gelling sugar batch. Recipe parameters Soluble solids content: 41% pH-value in

Recipe parameters

Soluble solids content: 41%

pH-value in final product: 3.20 ± 0.05

Buffer solution: Potassium citrate / citric acid

buffer solution

Pectin dosage: 0.30% – 1.05%

The determination of breaking strength is done

at 20° C, 2h after preparation of the gel.

strength is done at 20° C, 2h after preparation of the gel. 8 Fig. 4: Breaking

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Fig. 4: Breaking strength of a standard model gel in dependence from pectin dosage low methylester amidated pectin (41% ss, product pH-value 3.2, potassium citrate / citric acid buffer solution, pectin dosage 0.30% - 1.0%)

HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de

c) Apple juice jelly for assessment of high me-

thylester pectins (e.g. in product development)

Especially the determination of the breaking

strength of jellies is suitable for an objective

assessment of the firmness of gel preparations

close to practice as jellies do not contain any

solid components which could influence the

measurement negatively.

If the used fruits are crushed to very fine par-

ticles also the breaking strength of jams can be

determined. In this case it has to be considered

the smaller the fruit pieces resp. fibres, the bet-

ter reproducible the measured results.

When determining the breaking strength in such

recipes close to practice also the variations of

raw materials’ composition and differences

during processing have to be considered which

differences during processing have to be considered which may have an influence on the absolute meas-

may have an influence on the absolute meas-

uring result. Therefore the use of a suitable re-

ference is recommended.

The determination of the breaking strength in

gel preparations close to practice is especially

suited for product development and for com-

parative investigations.

Recipe parameters

Soluble solids content: 62%

pH-value in final product: 3.20 ± 0.05

Pectin dosage: 0.30% – 0.70%

The determination of breaking strength is done

at 20° C, 24h after preparation of the gel. In

order to avoid the drying of the surface, the

beakers are covered by a plastic film.

of the surface, the beakers are covered by a plastic film. 9 Fig. 5: Breaking strength

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Fig. 5: Breaking strength of an apple juice jelly in dependence from pectin dosage citrus pectin DE° 56%, 150° USA-Sag (62% ss, product pH-value 3.2 +/- 0.05, pectin dosage 0.30% - 0.70%)

TECHNICAL APPLICATION LABORATORY HERBSTREITH & FOX CORPORATE GROUP

09/06/2004

HERBSTREITH & FOX Corporate Group • Turnstraße 37 • 75305 Neuenbürg/Württ. • Germany Phone: +49 7082 7913-0 • Fax: +49 7082 20281 • info@herbstreith-fox.de • www.herbstreith-fox.de