T ECHNICAL A PPLICATION I NFORMATION

Herbstreith-Pektinometer Mark IV

I NTRODUCTION

The Herbstreith Pektinometer Mark IV is a further development of the Herbstreith Pektinometer Mark III which has already been established since more than fifteen years. It is used for the determination of breaking strength of gels, especially of pectin gels which are produced with high and low methylester pectins.

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 objective determination of the gelling behaviour of pectin gels in quality control as well as for

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 development.

product development.

Above all the request for an extended measuring range, for a timely and modern data recording and for a user-friendly and pleasing design finally lead to the development of the

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 Lochmller. 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.

Herbstreith Pektinometer Mark IV.

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.

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. 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 standardised shear insert out of a standardised measuring beaker being filled with a defined gel in order to disrupt the gel.

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

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 K are comparably high.

Constant measuring conditions during the disrupting procedure are the precondition for reproduceable results. They are assured at the Herbstreith Pektinometer Mark IV by the following 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 Elastic viscous, i.e. very smooth and spreadable 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 progression of the force-time-curve additionally gives information concerning the consistency (texture) of the gels. Therefore the Herbstreith Pektinometer Mark IV records the force progression during the disrupting procedure and assesses it. From the quotient of maximum force (HPE) and integral of the force-time-curve the socalled texture constant K is determined with which a conclusion concerning the gels texture becomes possible. Fig. 2: Force-time-diagram of an elastic-viscous gel Fig. 1: Force-time-diagram of an elastic-brittle gel

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. 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 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 Speed of extension: Distance of extension: Measuring distance: Measuring range: Measuring exactness: Technical data Measuring value uptake: DMS measuring stirrup uptak with amplifier 20 g 3000 g 1% from measuring value, < 5 HPE 10 mm/s 60 mm 30 mm

Key control elements of the Herbstreith Pektinometer Mark IV are the user-friendly LCD display 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 purpose the Herbstreith Pektinometer Mark IV records each final 500 files.

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. 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 with the Herbstreith Pektinometer Mark III is a method which has been widespread since many years. Therefore the new Herbstreith Pektinometer Mark IV has been conceived that way that it provides values comparable to the former model at simultaneously improved measuring technique. The extension speed of 10 mm/s is controlled 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. Also the extension force is already calibrated from the producer for the whole measuring range so that an after-adjustment is no more A new property of the Herbstreith Pektinometer 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. necessary. A control of the extension force e.g. within control of inspection, measuring and test equipment can be done with suitable standardised weights. Then the thermo printer prints a check protocol stating the measured Additionally the Herbstreith Pektinometer Mark IV offers the possibility to characterize the texture of the gels, i.e. the elastic resp. elastic viscous properties by means of the texture constant K which is issued with each measuring protocol. value as well as the mass of the used standardised weight. by the gear motor also under load and does not have to be checked or adjusted. 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. With that the user has the possibility to process the measuring values by pc connected to the ethernet resp. to record them digitally.

Furthermore the Herbstreith Pektinometer Mark IV possesses an internal memory which is conceived for recording each final 500 files.

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. 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 quality control and product development. In contrast to that the pectin gels are charged For the standardization of high and low methylester pectins traditionally the so-called ridgelimeter method is used. This method describes the production of a pectin-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). 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 Pektinometer corresponds to the impression of the consumer which is noticed as sensoric gel strength. This internationally accepted method distinguishes itself primarily by its simple handling and good reproducibility. For determination of the gel strength by means of breaking strength with the Herbstreith Pektinometer Mark IV almost user-defined recipes 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 measurement and obtaining results. (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 necessary that the produced gel preparations gel and that fruit components if they are used are grinded fine resp. show a relatively small As gels being produced according to the ridgelimeter method are not becoming destroyed during the measuring this method basically detects elastic properties which do not always particle size and are distributed homogeneously. 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. correlate with the real inner firmness, i.e. breaking strength.

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. 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 possible to characterize high methylester, low methylester and high resp. low methylester, amidated pectins by the determination of breaking strength over a relatively wide ss and pH range.

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 pectins in the field of incoming goods inspection or quality control often standard model gels are

Furtheron by suitable recipe selection the results of the breaking strength determination by using the Herbstreith Pektinometer Mark IV can be already obtained after very short standing time of the gel (e.g. after 2h).

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 preparation is replaced by a suitable buffer solution.

As especially in the field of quality control reproducible results are quickly requested and in the field of product development the assurance of sensoric impressions by means of objective measurements is required, the determination of the breaking strength with the Herbstreith Pektinometer Mark IV is a reasonable and necessary supplementation to the ridgelimeter method.

With that it is possible to exclude quality variations caused by the fruits. The obtained breaking strength correlates with the firmness which the pectins will reach in jams and jellies.

Recipe parameters Soluble solids content: 65% pH-value in final product: 3.10 0.05 Buffer solution: Potassium acetate / lactic acid

This is demonstrated with three typical applications in the following.

buffer solution Pectin dosage: 0.100% 0.275%

The determination of breaking strength is done at 20 C, 2h after preparation of the gel.

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%)

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. 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)

Recipe parameters Soluble solids content: 41% pH-value in final product: 3.20 0.05 Buffer solution: Potassium citrate / citric acid

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.

buffer solution Pectin dosage: 0.30% 1.05%

The determination of breaking strength is done at 20 C, 2h after preparation of the gel.

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.

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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%)

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. 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 methylester pectins (e.g. in product development)

may have an influence on the absolute measuring result. Therefore the use of a suitable reference is recommended.

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. Recipe parameters If the used fruits are crushed to very fine particles 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 better reproducible the measured results. The determination of breaking strength is done at 20 C, 24h after preparation of the gel. In 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 order to avoid the drying of the surface, the beakers are covered by a plastic film. Soluble solids content: 62% pH-value in final product: 3.20 0.05 Pectin dosage: 0.30% 0.70% The determination of the breaking strength in gel preparations close to practice is especially suited for product development and for comparative investigations.

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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

H ERBSTREITH & F OX Corporate Group Turnstrae 37 75305 Neuenbrg/Wrtt. Germany Phone: +49 7082 7913-0 Fax: +49 7082 20281 info@herbstreith-fox.de www.herbstreith-fox.de