Food analysis

Quality control in the food and beverage industry

02

Metrohm...

• is the global market leader in titration

• is the only company to offer a complete range of ion analysis equipment – titration,
voltammetry and ion chromatography
• is a Swiss company and manufactures exclusively in Switzerland
• grants a 3-year instrument warranty and a 10-year warranty on chemical suppressors for
ion chromatography
• provides you with unparalleled application expertise
• offers you more than 1300 applications free of charge
• supports you with expert service through local representatives and regional support centers
• is not listed on the stock exchange, but is owned by a foundation.
• gives the interests of customers and employees priority over maximizing profit
Metrohm – customized analysis for the food and
beverage industry
The law sets high standards
The food industry is subject to particularly strict regula-
Count on our support
As a leading manufacturer of instruments for chemical
03
tions on the quality and safety of its products. This is not analysis, we are quite aware of these challenges you
without reason: If contaminated food reaches the retail face. For this reason, we offer you not just the most
market, the consequences can be serious – and not just advanced equipment, but rather complete solutions for
for the consumers. the particular tasks at hand. Your partners at Metrohm
are experienced professionals who develop customized
Regulatory compliance applications for you and support you in every aspect of
In order to guarantee the industry’s strict quality and regulatory compliance with our expert service.
safety standards, reliable instruments and methods are
needed in the laboratory. These instruments and meth- On the following pages, discover the solutions Metrohm
ods must meet highest standards. Regulatory compliance offers the food industry in general and you in particular,
is the catchword here. to ensure the quality and safety of your products.
Challenge us!

Metrohm instruments comply with numerous official

standards, including the FDA regulation Title 21 CFR
Part 11.
 Methods available from Metrohm for the food
industry

04 The following table is organized according to product

areas and lists relevant parameters that can be deter-
important for you, please contact your local Metrohm
representative. We are continuously expanding our range
mined using methods developed by Metrohm. Moreover, of applications and will gladly assist you in solving your
you can see which standards these methods fulfill. If you specific analytical problem.
cannot find your sample matrix or a parameter that is

Sample Parameters Parameters Parameters Parameters Parameters

for titration for voltammetry for stability for ion chromatography for ProcessLab
measurement
Meat products, meat Chloride (NaCl) Pb in fish - Anions: nitrite, nitrate Chloride (NaCl)
extracts, bouillon Kjehldahl nitrogen (AOAC 972-24) (DIN EN 12014-4:2005), chloride,
preparations, spices, Sulfurous acid phosphate
soups, sauces - Polyphosphates
- Organic acids
- Cations: Na+, NH4+, K+, Ca2+,Mg2+,
- Biogenic amines in fish
- Monosaccharides and
disaccharides
- Sugar alcohols
Table salt, spices, Chloride (NaCl) Iodide, iodate - Anions: sulfate, sulfite, bromide, Chloride (NaCl)
pickling salt, herbs Total iodine iodide, chloride, iodate, fluoride, Total iodine
and aromatic salts Fluoride phosphate, molybdate Fluoride
Tricalciumphosphate - Polyphosphates Tricalcium phosphate
Nitrite - Organic acids Nitrite
- Cations: Na+, K+
Canned fruit, Oxalic acid Sn, other heavy - Anions: phosphite, nitrite, nitrate Chloride (NaCl)
vegetables and mush- Total sulfurous acid metals (DIN EN 12014-2:1997), chloride,
rooms, dried fruit Acid content phosphate, sulfate, perchlorate
and vegetables Salt content - Organic acids
- Cations: K+, Mg2+
- Monosaccharides and
disaccharides
Sweeteners, gelling Methoxy and ethoxy - Anions: fluoride, chloride, bromide,
and thickening agents groups nitrate, phosphate, sulfate
Cyclamate - Organic acids
Saccharin - Cations: Na+, K+, NH4+, Ca2+, Mg2+,
Fe2+
- Mono-, di-, oligo- and
polysaccharides
- Sugar alcohols
- Glycerol
- Sucralose, saccharin, cyclamate
Coffee, cocoa, pH value and acidity - Anions: fluoride pH value and acidity
chocolate, tea Ash alkalinity - Organic acids Ash alkalinity
Chloride - Cations: Na+, K+, Ca2+, Mg2+ Chloride
Direct reducing - Monosaccharides and Direct reducing sugars
sugars disaccharides in instant coffee Free fatty acids
Kjehldahl nitrogen (ISO 11292) Iodine value
Free fatty acids - Arabinose, fructose, galactose, Saponification value
Iodine value glucose, mannose, sucrose, xylose,
Saponification value maltose, lactose
- Sugar alcohols
- Glycerol
- Caffeine
Beer, vinegar, spirits pH value and total Heavy metals - Anions: fluoride, chlorite, chloride, pH value and total acid
and wine acid (Cd, Pb, Cu, ...) bromide, nitrate, sulfite, sulfate, CO2 content
CO2 content (Swiss Fruit Assn.) phosphate, oxalate Ascorbic acid
Ascorbic acid - Organic acids Free and total sulfurous
Free and total - Cations: Na+, K+, NH4+, Ca2+, Mg2+ acid
sulfurous acid - Transition metals: Cu2+, Zn2+, Fe2+, Volatile acids
Volatile acids Mn2+ Chloride
Ash alkalinity - Biogenic amines Sulfate
Chloride - Monosaccharides, disaccharides Total ester content
Sulfate and oligosaccharides
Total ester content - Sugar alcohols
- Glycols
Sample Parameters
for titration
Parameters for
voltammetry
Parameters
for stability
Parameters
for ion chromatography
Parameters
for ProcessLab 05
measurement
Fruit and vegetable pH value and Ascorbic acid - Anions: chloride, phosphate, pH value and titratable
juices, fruit nectars titratable total acid Pb (AOAC 979-17) sulfate, nitrite, phosphite total acid
and jams Ascorbic acid Fumaric acid - Organic acids Ascorbic acid
Sulfurous acid (AOAC 968-16) - Cations: Na+, K+, Ca2+, Mg2+ Sulfurous acid (sulfite)
(sulfite) Saccharin - Monosaccharides and Chloride
Chloride (SLB 41-2.5) disaccharides Total phosphorous
Total phosphorous Sulfate
Sulfate Calcium and magnesium
Cations: Ca2+, Mg2+, Potassium
K+ Formol number
Ash alkalinity Reducing sugars
Formol number
Reducing sugars
Milk and dairy pH value and Pb (AOAC 974-13; - Anions: iodide, chloride,
products titratable acid AOAC 979-17) phosphate, sulfate, nitrate, nitrite,
Chloride thiocyanate, perchlorate, cyanurate
Calcium - Organic acids
Ascorbic acid - Cations: Na+, NH4+, K+, Ca2+, Mg2+
Kjehldahl nitrogen - Monosaccharides and
disaccharides
- Choline
- Melamine
Nuts Oxidation
stability
Fruit and vegetables Oxalic acid Zn (ISO 6636-1) pH value and titratable
Total sulfurous acid total acid
Chloride Ascorbic acid
(e.g., oranges)
Grains Cd, Pb (AOAC
983-23)
Animal and plant fats Acid value and free Oxidation - Anions: phosphate, bromate Hydroxyl number
and oils fatty acids stability (AOCS - Cations: Ca2+, Mg2+ Iodine value
Hydroxyl number Cd 1b-92, Peroxide value
Iodine value ISO 6886) Saponification value
Peroxide value Native olive oils:
Saponification value Acid value
Free fatty acids
Water content
Crackers, baked Oxidation - Monosaccharides and
goods stability disaccharides
Instant noodles Oxidation
stability
Table and mineral pH value and acid U (DIN 38406-17), - Anions: fluoride, chloride, nitrite, Conductivity
water, drinking water capacities CN– (sample bromide, nitrate, phosphate, Alkalinity
Ca2+, Mg2+ and total preparation sulfate, iodide, silicate, carbonate, pH value and acid
hardness according to chromate capacities
Chloride, sulfate DIN 38405-13) ASTM D 4327-03 Ca2+, Mg2+ and total
Sulfides/hydrogen EPA 300.1 hardness
sulfide ISO 10304-1:2007 Chloride, sulfate
Total and residual - Oxyhalides: bromate, chlorite, Sulfides/hydrogen sulfide
chlorine chlorate Total and residual
Permanganate index ISO 10304-4 chlorine
CO2 content ASTM D 6581-08 Permanganate index
Oxygen content - Cations: Na+, NH4+, K+, Ca2+, Mg2+ CO2 content
according to Winkler ISO 14911:1998
- Phenols
Soft drinks Citric acid/citrate - Anions: chloride, nitrate, Acid content
Phosphoric acid phosphate
(cola drinks) - Organic acids
Potassium - Cations: Na+, NH4+, K+, Ca2+, Mg2+
Total phosphorus - Monosaccharides and
disaccharides
- Sugar alcohols
- Phenylalanine, aspartame, caffeine
- Glucoronolactone
Rinsing, cleaning and Ingredients in rinsing
disinfection processes and cleaning solutions,
in the beverage acids, such as peracetic
industry acid, pH value and
conductivity
 pH measurement

06 pH measurement is one of the most important parame-

ters in the quality control of foodstuffs. pH provides
information on the quality of natural products such as
citrus fruits, juices or dairy products for example.
Furthermore, pH is an important parameter in the use of
acidity regulators as preservatives.

The requirements of the pH electrode that is used for

measurement are just as varied as the many foods to be
analyzed. The selection of a diaphragm that is appropri-
ate for the sample is especially important since otherwise
the electrolyte bridge can quickly become blocked by the
sample, which leads to erroneous measurements.

The following table shows examples of which Metrohm

electrode is suitable for pH determination in which foods.

Sample Electrode Properties

(Order Number)
• Precise measurements and very rapid response even
in low-conductivity, weakly buffered solutions
• contamination-insensitive fixed ground-joint
Aquatrode plus
Drinking water diaphragm
(6.0257.000)
• Maintenance-free reference electrolyte, variable
outer electrolyte for special applications
• Optimized length for sample changer applications
General, e.g., wine and • Universal use
spirits, fruit and Unitrode • Short response time after temperature changes
vegetable juices, cereals (6.0258.600) • Contamination-insensitive fixed ground-joint
confectioneries diaphragm
• Especially for highly contaminated and protein-
Protein-containing samples Porotrode containing or viscous samples
(e.g., dairy products) (6.0235.200) • Low maintenance capillary diaphragm
• Polymer electrolyte for uniform electrolyte flow
• Robust electrode tip for measurements in semisolid
Penetration measurements Spearhead samples
(e.g., dough, cheese, meat) (6.0226.100) • Maintenance-free reference electrolyte
• Easy-to-clean pinhole diaphragm
Surfaces, small sample Flat membrane electrode • For measurements on surfaces or in very small
volumes (6.0256.100) sample volumes
 07

Rugged, reliable and easy to use: pH meters from

Metrohm
pH determinations with the 826 pH mobile and pH, chloride, fluoride and ammonium determina-
827 pH lab meters tions with the 780 pH Meter or 781 pH/Ion Meter
Whether you are performing routine pH determinations The 780 pH Meter is the top choice if you need to know
in the laboratory or out in the field – with Metrohm pH everything exactly: nine-point calibration, stirrer control,
meters you never have to do without GLP: three-point electrode test for glass pH electrodes, method memory
calibration, automatic buffer recognition, temperature and RS232 interface.
compensation, sample identification, GLP-compliant
printout and a large memory for storing measurement Besides measuring pH, the 781 pH/Ion Meter can also
results – pH meters from Metrohm offer all of these determine the concentration of individual ions (e.g., Cl–,
features at a very attractive price. F– and NH4+) by either direct measurement or fully auto-
matic standard addition.
 Titration

08 Benefit from the know-how of the market leader

Metrohm is the leading manufacturer in the field of titra-
An overview of some application examples

tion. Sixty years of experience and the most comprehen- Total sulfurous acid in dried fruits SLMB 553.1
sive and innovative program on the market are proof of Iodine value of edible fats and oils AOAC 28.023
our strength. Our collection of potentiometric applica- Sulfurous acid in wine AOAC 940.20
tions that is available to you is huge. Benefit from more pH value of beer AOAC 945.10
than 150 proven titration applications from the food Total hardness of drinking water EPA 130.2
industry sector that we have prepared based on the Salt (NaCl) in meat and meat products AOAC 935.47
following publications: Total acid in nonalcoholic beverages AOAC 950.15
Acidity of roasted coffee beans AOAC 920.92
• Deutsche Einheitsverfahren zur Wasser-, Abwasser Oxalic acid in fruit and canned fruit AOAC 974.24
and Schlammuntersuchung (German Standard Ascorbic acid (vitamin C) AOAC 967.21
Methods for the Examination of Water, Wastewater
and Sludge)
• Official Methods of Analysis of the Association of
Official Analytical Chemists (AOAC, U.S.A.)
• Schweizerisches Lebensmittelbuch (SLMB; Swiss
Manual on Food Safety)
• U.S. Environmental Protection Agency (EPA)

Electrodes for titration

The correct electrode for every application

Choosing the right electrode is crucial for successful titra- This is the case for many applications in the food indus-
tion. For combined electrodes, the correct diaphragm try. If the electrode reacts too slowly, the solution will be
must be chosen because otherwise the electrolyte bridge over-titrated and incorrect results are obtained. Metrohm
can become blocked. The response behavior of the elec- offers an appropriate electrode for every need. The fol-
trode is also important, in particular if the titration is to lowing table shows which Metrohm electrode is suitable
be carried out to a defined endpoint. for which application.

Area of application Metrohm electrode

General Ecotrode plus 6.0262.100
Acid content of alcoholic beverages Unitrode 6.0258.600
Carbonate hardness, acid capacity of water, p and m values Aquatrode plus 6.0257.000
Determination of Ca2+, Mg2+ (complexometric) 2+
Ca ISE 6.0508.110
Permanganate index Pt Titrode 6.0431.100
Titratable total acid in dairy products Porotrode 6.0235.200
Calcium content in dairy products Cu2+ ISE 6.0502.140
Kjehldahl nitrogen in milk Ecotrode Gel 6.0221.100
Vitamin C in fruit juice Double Pt-sheet electrode 6.0309.100
Formol number Unitrode 6.0259.100
Free fatty acids, hydroxyl number in oils Solvotrode 6.0229.100
Iodine value, peroxide value Pt Titrode 6.0431.100
Water determination according to Karl Fischer Double Pt-wire electrode 6.0338.100
General chloride, table salt content in food Ag Titrode 6.0430.100

Additional examples and practical tips on using Metrohm Titration» and «Electrodes for pH Measurement». These
electrodes are given in the leaflets «Electrodes for can be downloaded for free at www.metrohm.com.
 Titration with Metrohm: Solutions for every need
and budget
09
With the 848 Food/Beverage Titrino plus, the 862 Food/
Beverage Compact Titrosampler and the 905 Food
Titrando, Metrohm offers you three complete titration
packages. No matter which package you choose, simple
and reliable work is guaranteed:

• intelligent exchange or dosing units ensure the use

848 Food/Beverage Titrino plus – the economically priced of the correct titration solution and permit their moni-
titrator for routine analysis in the food laboratory. This all-inclu- toring
sive package also comprises an USB stick with 100 methods
• all important titration parameters are stored with the
stored for the most important applications in food analysis.
methods; this means that even unskilled users quickly
obtain reliable results
• GLP-compliant data output either on a printer or by
digital archiving

862 Compact Titrosampler – the automatic titration station

for higher sample throughput. With the 862 Food/Beverage
Compact Titrosampler and the 862 Salt Compact Titrosampler,
Metrohm offers two all-inclusive packages that come with
everything from the electrode and sample beaker to the method
templates for the professional food analysis.

905 Food Titrando – the high-end titrator for the highest

demands. Frequently used methods can be started with the
push of a single button. Complete traceability of measuring
results, central data management through the client-server
option, method templates, individual method development,
possibility for complete automation and much more.
 Thermometric titration: the ideal complement to
potentiometric titration

10 Thermometric titration is a highly versatile determination

method and is the ideal complement to potentiometric
This principle is the basis of thermometric titration. In a
thermometric titration, reagent solution (titrant) is con-
titration. In principle, the method is suitable for every tinually added until the endpoint is reached. The end-
reaction that creates a sufficiently large temperature point is seen as a break in the titration curve if the tem-
change in the sample solution. This method is particu- perature is plotted as a function of the volume of added
larly suitable in applications for which: titrant.

• an appropriate potentiometric sensor is not available

• an appropriate reference electrode is not available
• the sample matrix would compromise or even destroy
the electrode
• an appropriate solvent for potentiometry is not available

Thermometric titration – the principle

Every chemical reaction is associated with a change in
reaction enthalpy. This results in either an increase (exo-
thermic reaction) or a decrease (endothermic reaction) of
the sample solution temperature.

859 Titrotherm
The 859 Titrotherm combines innovative, glass-free
sensor technology and the unrivalled titration know-how
of Metrohm. The instrument is automatically recognized
when connected to a computer and hence, must not be
manually configured. The software determines the end-
points based on the first and second derivatives of the
titration curve; with additional optimization parameters,
reproducibility can be further increased.

Advantage of thermometric titration: The temperature sensor (thermoprobe) of the 859 Titrotherm is almost maintenance-
free and can be used immediately without prior conditioning.
 11

Application examples
Unsaturated fatty acids in edible oil Determination of sodium content in food
Determination of the content of unsaturated fatty acids The sodium content of foods is usually determined indi-
in edible oil is based on the titration of weak acids in rectly through a precipitation reaction with silver nitrate.
nonaqueous solutions with a dilute solution of a strong For this, it is assumed that the chloride and sodium ions
base in alcohol. Problems that occur when performing are in a 1:1 molar ratio. However, this is not true if other
potentiometric titrations on samples with low free fatty chemical substances such as sodium benzoate and mo-
acid contents can be avoided with thermometric titra- nosodium glutamate or compounds such as potassium
tions. Thermometric titration is simple and employs a chloride that contain sodium chloride are present in the
catalyzed indicator reaction. matrix. This is often the case for sodium-containing foods.

Established methods for the direct determination of so-

dium such as AAS or ICP/MS have the disadvantage that
the required instruments are very expensive. Thermo-
metric titration is a cost-effective and easy-to-perform
alternative. To carry out this method, the sample is first
homogenized. Afterwards, the sample solution is titrated
with an aluminum nitrate solution containing an excess
of potassium ions in the presence of NH4HF2 at pH 3.
Insoluble NaK2AlF6 is formed in an exothermic reaction.
 Karl Fischer titration

12 Determination of water content in food,

beverages, tobacco and pet food
When to determine water volumetrically,
when coulometrically?
The water content largely determines the quality and The water content of food varies considerably. The water
shelf life of many food products. The amount of water in content of beverages varies between 40 and 98%. Be-
food can be easily determined by means of Karl Fischer cause of these high water contents, weighing out the
titration. sample directly into the titration vessel is not feasible
since the weighing error for small samples would be too
Water exists in food in different forms. They range from large. Such samples are pre-diluted with methanol and
clearly defined forms (for example, as in sucrose and measured by volumetric Karl Fischer titration. In contrast,
alcoholic beverages) to those in complex cellular struc- pure fats and oils are measured preferably coulometri-
tures (for example, as in dry fruits) in which the water is cally due to their low water content.
bound to the surface as well as between particles.
Moreover, water can also be trapped within the cells and Very few side reactions
must be released through appropriate sample prepara- In foods, very few chemical side reactions that release
tion before the measurement. water or react with iodine are expected. Substances such
as aldehydes and mercaptans are present in only small
Simple sample preparation amounts if at all; their amounts can be disregarded in
For the latter types of samples, the use of a high fre- view of the usually high amounts of water present.
quency homogenizer is recommended. Homogenizing
releases the water and at the same time, stirs the sample. However, should side reactions occur, the oven method
Because the sample preparation takes place directly in is an alternative. The sample is weighed into a vessel,
the titration vessel, no additional water is absorbed and which is then sealed airtight. Afterwards, the sample is
the water content determined is not biased. heated and the moisture transferred with a stream of dry
carrier gas to the titration cell, where the actual water
In most food, water is not distributed homogeneously determination takes place. Because the sample does not
throughout the material. The sample to be measured enter the titration cell, side reactions do not occur.
must be taken so that it statistically represents the aver-
age. To this end, a larger amount of sample (if necessary)
is comminuted and homogenized and the water content
determined in an aliquot.
Application examples
The following table shows by which technique various titration procedures can be found in the free Metrohm
13
foodstuffs can be analyzed. Detailed information and monograph «Water Determination by Karl Fischer Titration».

Samples Type of Titration

Non-alcoholic beverages Fruit juices, vegetable juices, syrups, soft drinks vol.
Frying fat, deep-frying, olive, peanut, sunflower canola and
Fats and oils coul.
safflower oils (AOAC 984.20, ISO 8534)
Dairy products, protein- Butter, milk, cream, yoghurt, cream cheese, curd cheese, cheese,
containing products, milk powder, yeast, mayonnaise, egg yolk, protein, gelatin, vol.
meat products meat, meat products
Honey, molasses, sugar Various sugars vol.
Candies, fruit gums, gumdrops, caramel, chewy candy, licorice
Confectionery vol.
sticks, toffee, gummi bears, marzipan, chewing gum, jam
Cognac, gin, fruit brandy, liqueur, whiskey, wine, chocolate,
Semi-luxury food
cocoa beans, cocoa powder, (AOAC 997.10), (instant coffee
(alcohol, coffee, tea,
(ISO 20938), roasted coffee beans, green coffee ISO 11817), vol.
cocoa, tobacco,
cappuccino powder, tobacco, pipe tobacco, cigarette tobacco
chocolate, spices)
(ISO 6488)
Nuts, dry fruits, Dry fruits (AOAC 967.19), dried fruit, nuts, almonds, dried
vol.
dried vegetables vegetables
Fruit and vegetables Various fruits and vegetables vol.
Barley, semolina, corn, rye, rice, soybean meal, wheat, cracked
Grain products and
wheat, potato and rice starches, cornstarch, soy and wheat flours, vol.
starch
glucose syrup, natural gums, breakfast cereals, oatmeal, popcorn
Baked goods, breads Noodles, breadcrumbs, zwieback, bread, cakes, crackers,
vol.
and pasta cookies, potato chips
Seasoning mixtures, potato flour, mashed potatoes, baby food,
Spices, other food vol.
instant soup, packaged soup mix
Pet food Canned pet food, fish meal, dog biscuits, flaked dog food vol.

901 Titrando plus Polytron: The samples are pulverized 874 Oven Sample Processor plus 852 Titrando: Place
or homogenized directly in the titration cell. Thus, additional sample vial on the rack, set the temperature, and water content
moisture cannot be absorbed during sample preparation. determination can begin. With the 852 Titrando, you can carry
This guarantees unbiased results. out both volumetric and coulometric titrations.
 Laboratory automation

14 The complete range of automatic sample

preparation from a single supplier
Normally, for determining pH, total acid or chloride con-
tents in liquid foods, accurate pipetting and dilution of
the sample is sufficient. Metrohm offers you a wide
range of products for the fully automatic preparation of
liquid samples.

On the other hand, if you are dealing with solid samples,

such as meat, fish, salads, jams or confectioneries to
name a few, sample preparation is more demanding. As
a specialist in laboratory automation, we offer you many
solutions for the fully automatic preparation of solid
samples, too.

Automation = time savings and higher accuracy Fully automatic titration of a homogenized sample:
With the 815 Robotic Titration Soliprep, sample preparation
In food and pesticide analysis, primarily chromatographic
and titration can be completed in one process without lling
methods such as IC, HPLC and GC are employed in out multiple copies of sample tables or shifting beakers around.
addition to direct titration. These techniques require that Mix-ups are prevented and standing time before analysis is
the sample is available as a filtered liquid before it can shortened.
be injected into the column. If carried out manually, pre-
paration steps such as

• pulverization / homogenization
• filtration
• pipetting / dilution

are tedious and time-consuming. Furthermore, manual

sample preparation always comes at the risk of biased
results. In particular, for high sample throughput and if
several different people are involved, consistent sample
preparation quality can hardly be guaranteed.

The 815 Robotic Filtration Soliprep

 Robotic Soliprep – automatic sample preparation
tailored to you needs
15
With instruments of the Robotic-Soliprep-family, devia-
tion in results and time-consuming manually performed
routines are no longer an issue. The solid substance is
just weighed out and placed in the sample rack – every-
thing else is done completely automatically. Depending
on the model selected, different steps can be combined
– including the direct connection to a chromatograph or
the the titration of the homogenized sample.

Robotic Robotic Robotic Robotic

Titration Filtration Flexible Soliprep
Soliprep Soliprep Soliprep for LC
Homogenization + + + +
Fully automatic ltration: The 815 Robotic Filtration Soliprep Titration +
lters away remaining solid matter from the homogenized Filtration + + +
sample. A clear ltrate is the result that can be either directly Filling
+
injected into an analytical instrument or further diluted. HPLC/GC-Vials
Connection to
+
a LC system
 Oxidation stability

16 A proven method
Oxidation stability characterizes the resistance of oils and
743 Rancimat – analyze up to eight samples at
the same time
fats and of fat-containing foods to oxidation. It is a Determination of the oxidation stability of oils and fats is
standard parameter of quality control in the production the classic application for the 743 Rancimat. In addition
of oils and fats in the food industry or for the incoming to vegetable oils and fats, fats of animal origin can also
goods inspection in processing facilities. be analyzed for oxidation stability using the 743 Rancimat.

For the determination of oxidation stability, a stream of Just as the pure substances oils and fats contained in
air is passed through the oil or fat sample at elevated foods are subject to oxidation, which contribute to food
temperature. This causes the oxidation of fat molecules spoilage. The 743 Rancimat can also be used to deter-
in the sample to volatile organic compounds and other mine the oxidation stability of fats and oils in foods.
products. The air stream carries these compounds to a
second vessel containing distilled water. The conduc-
tivity of the water is continuously recorded. The time
elapsed until these reaction products are formed and
detected is called the induction time or Oil Stability Index
(OSI).

The 743 Rancimat permits the determination of oxidation stability in accordance with international standards. The software for
recording and archiving the data in a data base with automatic analysis of the curves is included with the instrument.
 17

Application examples
Oxidation stability of fats and oils Oxidation stability of nuts
If fats and oils are exposed to air and light for any length The microstructure of the fresh, intact nut prevents rapid
of time, they undergo oxidation and hydrolysis reactions. oxidative spoilage. This microstructure is destroyed dur-
The fats and oils then develop an unpleasant taste and ing the processing of nuts. As a result, fat oxidation is
odor and are termed rancid. Oxidation stability is an accelerated and the shelf life shortened. Before the oxi-
estimate of how quickly a fat or oil will become rancid. dation stability of nuts can be determined, the fat-con-
Through the use of the 743 Rancimat, it is also possible taining phase must be separated from the rest of the nut
to characterize the efficacy of added antioxidants. with petroleum ether. The isolated fat is analyzed in the
743 Rancimat.
Oxidation stability of instant noodles
An example of an application for the 743 Rancimat is the Oxidation stability of crackers or other baked
determination of the oxidation stability of instant noodles. goods
The noodles are deep-fried during the manufacturing The Rancimat method is a simple method for determin-
process to make preparation by the consumer faster. Due ing the oxidation stability of fats contained in cereals,
to the deep-frying step, instant noodles have a high fat crackers, biscuits and other baked goods.
content (up to 22%) and hence can become rancid after
some time.
 Ion chromatography

18 Ion chromatography (IC) is a standard method for food

analysis. Numerous main ingredients, minor ingredients
Save time and costs through automatic sample
preparation
that affect taste and nutrition as well as traces of con- As in titration, sample preparation in ion chromatogra-
taminants can be reliably and precisely determined by IC. phy is an important factor. Novel inline methods (some
patented by Metrohm) permit the integration and com-
Multicomponent determinations in a single plete automation of sample preparation into the analyti-
analysis cal process. This increases safety, reduces the number of
In addition to anions and cations, carbohydrates, organic manually performed steps, improves reproducibility and
acids and polar substances can also be quantified in a guarantees the traceability of the entire analysis (includ-
variety of foods or drinks. The advantage of ion chroma- ing sample preparation).
tography is that chemically similar substances can be
determined in parallel in a single analysis. Furthermore, Metrohm inline sample preparation methods for food
the concentration of the analytes can vary from ng/L up analysis:
to the percent range. Of course, all Metrohm IC instru-
ments and the MagIC NetTM chromatography software • Inline Ultrafiltration
comply with FDA regulations. • Inline Dialysis
• Inline Dilution
• Inline Extraction
• Inline Matrix Elimination
• Inline Enrichment
• Inline Degassing
• intelligent Partial Loop Injection

Inline Ultraltration reliably removes interfering particles from the sample solution
and thus protects the separation column from contaminations.
Application examples
Analysis of mineral water
19
The anionic and cationic substances in table and mineral
waters are analyzed by IC. National standards set binding
limits for harmful ions such as bromate. The German
drinking water ordinance originally stipulated a limit of
25 g/L for bromate, but lowered it to 10 g/L in 2008.
The limit for mineral water is 3 g/L. The EU and the U.S.
Environmental Protection Agency (U.S. EPA) have set the
same maximum bromate concentrations for their drink-
ing water guidelines.

Other ions such as iodide affect the taste of water and

for this reason, are monitored in mineral water as quality
parameters.

Analysis of a mineral water sample spiked with 2 g/L bromate

in the 844 UV/VIS Compact IC with post-column derivatization;
Column: Phenomenex Star Ion A300 HC; eluent: 100 mmol/L H2SO4,
0.0193 mmol/L (NH4)6Mo7O24·4H2O, 0.7 mL/min; injection volume:
1000 L; post-column reagent: 0.27 mol/L KI; UV detection:
352 nm; Inline Degassing and Inline Ultraltration.

844 UV/VIS Compact IC with 838 Advanced IC Sample Processor. The ideal
system for photometric determination of polar substances, anions and cations in the
UV/VIS range.
20 Analysis of dairy products
For dairy products – be it baby food, yoghurt, milk or reagent. Ion chromatography permits the determination
lactose-free foods – ion analysis is essential to quality of anions (e.g., iodide, chloride, phosphate, sulfate,
control. Inline Dialysis is an efficient sample preparation nitrate, nitrite, thiocyanate, cyanurate and perchlorate),
technique for fully automatic removal of protein-contain- cations (e.g. sodium, ammonium, potassium, calcium,
ing matrices. Hence, it replaces the time-intensive, manu- magnesium and melamine) and also carbohydrates e.g.,
ally performed protein precipitation step with Carrez galactose and lactose).

Anion analysis of ultra-high temperature processed milk. IC with

conductivity detection; column: Metrosep A Supp 5–100; eluent:
3.2 mmol/L Na2CO3, 1.0 mmol/L NaHCO3, 0.7 mL/min; column
temperature: 30 °C; injection volume: 20 L.

Inline Dialyse – the ideal inline sample preparation for the

removal of proteins, oils and particles prior to ion chromato-
graphy.

881 Compact IC pro with 858 Professional Sample

Processor and 800 Dosino dosing system for ion analysis with
integrated Inline Dialysis.
 21

Carbohydrate analysis
How sweet is sweet? This question cannot be directly that can be reliably analyzed by ion chromatography and
answered for many foods. The following table shows pulsed amperometric detection (PAD). The type of sample
numerous sugar components in different food matrices preparation is also given.
Sample Preparation

Propylene glycol

Maltopentaose

Maltoheptaose
Maltohexaose
Maltotetraose
Maltotriose
Matrix
Cellobiose
Arabinose

Galactose

Rafnose
Mannose
Mannitol

Fructose
Glycerol

Maltose
Glucose
Sorbitol

Sucrose
Lactose
Inositol

Ribose
Xylose
Xylitol

Potato extract P, D, F + + +
Functional food P, D, F + + + + + +
Food extracts P, D + + + + +
Dairy products Dialysis + + + + + + + + +
Baby food Dialysis + + + +
Instant tee D, F + + + +
Beer U, D +
Beer wort F, D + + + + +
Malt extract D + + + + + + +
Vodka D + + +
Apple juice D +
Cola D + + +
Diet cola D + + + +
Orange juice D, F + + + +
Instant coffee E, D, F + + + + + + + +
Red beet extract D + + + + + + + + + +
Corn syrup D + + +
Maple syrup D + + +
Sugar-free chewing gum E, D, F + + + +
Candies E, D, F + + + + +
Chocolate E, D, F + + + + + + + + + + +

Polyols, sugar alcohols, monosaccharides, disaccharides, oligosaccharides

P: Pulverization, D: Dilution, E: Extraction, F: Filtration, U: Ultrasonic treatment
 Voltammetry

22 High detection sensitivity for a low price

Voltammetry is an electrochemical analytical method to analysis. Several organic substances in food, for example,
that provides information on the type and amount of vitamin C, vitamins of the B group or quinine, can also be
substances contained in a dissolved sample on the basis determined by voltammetry.
of a current-voltage relationship. The importance of vol-
tammetry lies in its high accuracy and sensitivity, the 797 VA Computrace
possibility of performing a speciation analysis and its The 797 VA Computrace is a state-of-the-art, computer-
favorable price-performance ratio. assisted voltammetric analysis system. The potentiostat/
galvanostat built into the instrument guarantees highest
Heavy metal ions that are present as contaminants in precision with reduced noise. The included PC software
food can be determined with high sensitivity by voltam- controls the determination and calculates and archives
metry. To this end, food samples must be digested prior the results.
 23

Application examples
Cd, Pb and Cu (also Zn, Ni, Co, Cr, Fe, etc.) in Vitamin C in fruits, vegetables and juices
wine and other foods Commercially available fruit and vegetable juices can be
The analysis of heavy metals in wine and other foods directly and straightforwardly analyzed as liquid samples.
provides information on the type and concentration of Likewise, freshly pressed fruit juices can also be directly
contaminants. In view of the importance of heavy met- analyzed. Beverages containing carbon dioxide should be
als, the exact determination of these elements by high- degassed prior to analysis.
performance methods is essential. With the 797 VA
Computrace, it is possible to perform the determination Tin in canned foods
of heavy metals in wine and other foods after UV diges- The metal used for making food cans is tin-plated steel
tion. which is then coated with plastic. If the plastic coating is
omitted, acid-containing foods in combination with
atmospheric oxygen can cause the tin to dissolve from
the can metal and diffuse into the food. Tin, which is
poisonous, can be determined with the 797 VA
Computrace.

Iodide in table salt

Iodine is an important trace element for the human body
and is added to table salt to prevent deficiency symp-
toms. Both iodide and iodate can be simply determined
Voltammetric determination of Cd, Pb and Cu in wine by voltammetry using the 797 VA Computrace.
 Atline process analysis with ProcessLab

24 Process control in food production

It is a long way before a raw material becomes a finished
ProcessLab – rugged and flexible design
This is exactly what the Metrohm ProcessLab makes pos-
product in the food industry. Numerous production sible – a robust and simple-to-operate analysis system
steps, such as pulverization, filtration, fermentation as that is set up directly on the production floor. The sample
well as heating, cooking, pasteurization, sterilization or is brought to the Process Lab and the analysis started by
distillation, are involved in the preparation of a product the push of a single button. The system is based on
and to make it storable. proven Metrohm titration and voltammetric compo-
nents. ProcessLab features a modular design; it is config-
In addition to the statutory final inspection and testing, ured to meet the user’s particular requirements and can
control of the different production steps also has an be optimally integrated into process communications
important role, which is to maximize throughput and through inputs and outputs (typically 4...20 mA). Only a
yield of a product. Valuable time is lost if the product few minutes after taking the sample, the relevant process
cannot be further processed or packaged while samples information is available to a LIMS or the master display.
from the various production steps are being tested in the
laboratory. It is thus a great advantage if these analyses Thus, ProcessLab is ideally suitable for rapid and inde-
can be performed directly at the process site while pro- pendent process control in the production environment.
duction goes on uninterrupted. A ProcessLab system consists of a TFT operating panel
with touch screen and an analysis module that is tailored
to the particular application. Due to its splashproof hous-
ing (protection class IP54), ProcessLab is well-suited for
use in harsh production environments.

ProcessLab system with operating panel and analysis module: Each system is congured with the relevant modules according
to the user’s particular requirements.
 25

Application examples
Determination of iodate and fluoride in table salt Determination of table salt in instant soups
production Table salt is an important flavor enhancer in the food
Iodized und fluoridated table salts are subject to strict industry and is used in numerous products. In the manu-
statutory regulations and require very careful monitoring facture of instant soups, it is important that the table salt
of the additives. The analysis of these parameters can be concentration in the finished product is exactly in accord-
performed directly on site with ProcessLab, which means ance with the specifications. Additionally, the crude salt
that the table salt can be immediately processed without used in the manufacturing process is subject to an in-
costly temporary storage. This increases throughput and coming goods inspection.
lowers production costs. Moreover, automated sample
preparation means higher reproducibility and compliance ProcessLab covers this broad range of applications in a
with statutory regulations can be more accurately con- single system permitting quality control of the complete
trolled. All requirements for comprehensive documenta- manufacturing process. Specifications for the documen-
tion and traceability of single batches are fulfilled. tation of the entire process are met.
 Online process analysis

26 Customized online process control

Production processes in the food industry must be con-
Straightforward network integration
All Applikon Analytical online analyzers come with digital
tinuously monitored. Online analyzers from Applikon and analog data outputs. Thus, e.g. results can be trans-
Analytical optimally fulfill this requirement. Engineered mitted via analog 4...20 mA signals and alarms triggered
for continuous operation, these instruments enable the by digital outputs. Or digital inputs can be employed for
fully automatic control of production processes – seven remote start/stop commands.
days a week, 24 hours a day. Moreover, it does not make
a difference whether a single parameter is to be deter- Robust design in stainless steel
mined in a single sample stream or several different para- Applikon Analytical analyzers are constructed for the
meters are to be determined in complex, multiple sample rigorous demands of the production environment. The
streams – the Applikon Analytical engineers provide you housings meets the specifications of NEMA 4 and protec-
with an appropriate system. tion class IP66. Applikon Analytical offers two instru-
ments with stainless steel housings, the ADI-201Y and
Proven wet chemistry methods the ADI-2040 Analyzers, for use in environments where
Applikon Analytical online analyzers are based on wet even tougher requirements for hygiene and durability
chemistry methods such as titration, colorimetry and apply, such as in the meat processing industry.
measurements with ion-selective electrodes. For these
methods, sampling and sample preparation are at least
as important as the analysis itself. Applikon Analytical has
great expertise in this field and configures the sampling
system to exactly fit your application including, e.g.
filtration, sample taking from pressurized containers or
degassing.

Applikon Analytical is a member of the Metrohm Group.

The company manufactures instruments for online analysis.

www.applikon-analyzers.com

ADI 201Y analyzer in stainless steel version for the food industry
 27

Application examples
Peracetic acid in beverage industry filling systems Sodium dihydrogen pyrophosphate in deep-
Peracetic acid is used in the beverage industry to sterilize frozen potato products
bottles before filling. Too much peracetic acid compro- Sodium dihydrogen pyrophosphate is added to blanch-
mises the taste of the beverage, requires more rinsing ing water during the production of deep-frozen french
and causes increased costs. On the other hand, if too fries to prevent a loss in color of the product. Too much
little peracetic acid is used, mold can start growing in the sodium dihydrogen pyrophosphate compromises the
bottles. Peracetic acid is determined by its reaction with taste of the product, while too little leads to a grayish
iodide through which elemental iodine is formed. The coloring. The determination of the sodium dihydrogen
iodine, in turn, can be determined colorimetrically. The pyrophosphate concentration requires thermal digestion
entire analysis including sample preparation can be auto- of the sample followed by colorimetric determination of
mated with an ADI 2019 analyzer. the orthophosphate content. Sample digestion and
analysis can be automated with the ADI 2040 analyzer.
Alkalinity of brewing water
The alkalinity of water is the overriding factor for decid- Salt and vinegar in mayonnaise
ing whether it is suitable for use as brewing water in the Salt and vinegar content are two of the most critical
production of beer. Whereas water with a high degree of parameters in the manufacture of mayonnaise. Both in-
hardness is only suitable for the production of bock beer, gredients not only affect the shelf life but also the taste
the brewing of lager beer requires soft water. Therefore, and consistency of the product. Whereas the vinegar
beer manufacturers must constantly monitor the hard- concentration can be determined by acid-base titration
ness of the brewing water. The alkalinity of water is (as glacial acetic acid), the salt content is determined by
determined by acid titration; the hardness of water is titration with silver nitrate. Both applications including
given in mg CaCO3 per liter. The ADI 2040 analyzer is sample taking and preparation can be easily automated
ideally suited for the fully automatic execution of this with on-line analyzers from Applikon Analytical.
important analysis.
 Service that you can rely on:
®
the Metrohm Quality Service

28 Reliable results for the lifetime of the analytical

instrument
Metrohm analytical instruments are engineered to deliver This includes:
extremely precise measurements. As a result, leading in- • competent assistance with Design Qualification (DQ)
ternational companies from the food industry also put • professional installation through compliant
their trust in us for our comprehensive services. These Installation Qualification (IQ)
services ensure that laboratory managers can rely 100% • Operational Qualification (OQ) guaranteeing that
on results produced during the entire lifetime of their Metrohm instruments meet the equipment
Metrohm analytical instruments. specification
• all qualification and validation work, which is
Regulatory compliance made easy performed only by professionally trained and certified
The food industry is required to comply with all effective Metrohm service specialists
laws and guidelines on food safety. Through Metrohm • user training taught by experts
Compliance Service®, we ensure that your company com- • competent requalification and revalidation
plies with standards such as IFS, BRC, SQF and ISO 22000.
If you want to put a Metrohm analytical instrument into
operation, we take care of everything else.
Why Metrohm Quality Service®?
®
The Metrohm Quality Service is available worldwide. service contract, for example, you can rely on the opti-
29
Preventive maintenance carried out on a regular basis mum performance of your Metrohm instruments at any
extends your instrument’s lifetime while providing for time, incur no additional costs whatsoever and benefit
trouble-free operation. All maintenance work done from complete and compliant verification documenta-
®
under the label Metrohm Quality Service is carried out tion. Thanks to our service, you are perfectly prepared for
by our own certified service experts. You can choose audits.
between different types of service contracts. With a full

An overview of Metrohm Quality Service®

Our Services Benefit for the Customer

Application support by means of our vast selection
of Application Bulletins, Applications Notes,
monographs, validation brochures, technical posters Quick and professional solution to all arising application
and articles questions and complex analytical challenges
Personal consultation by our specialists per telephone
or e-mail
Competent users contribute substantially to
Training courses
reliable results
Accurate measurements
Certified calibrations, for example of dosing and
Verification documentation for compliance with
exchange units
regulations and for efficient audits
Remote maintenance Expeditious resolution of software questions
Back-up support High data security
Short response times and thus, rapid problem resolution
Emergency service, for example express on-site repairs
Minimization of downtime
Original spare parts, made in Switzerland and available Lasting, successful repair; short delivery times
world wide Minimization of downtime
Guaranteed spare parts available for at least 10 years Protection of your investment through long-term
beyond instrument discontinuation date availability of spare parts and accessories
Decentralized repair workshops located around the Quality repairs done quickly, so your instruments
world and a central workshop in Switzerland are ready for use again

Thanks to Metrohm Quality Service®, you can rely on your results for the lifetime of the analytical
instrument. We look forward to a trustworthy partnership.
 Ordering information

30 pH Measurement
2.826.0110 826 mobile pH meter with carrying case and electrode
2.827.021x 827 pH lab IrDA with Unitrode
2.780.0010 780 pH Meter, high precision pH meter with Unitrode
2.781.0010 781 pH/Ion Meter with Unitrode
2.867.0110 867 pH Module with touch control
2.867.0210 867 pH Module with tiamoTM light

Titration
2.848.1010 Food/Beverage Titrino plus
2.136.0010 Titrotherm
2.848.1020 Food/Beverage Titrino plus with printer
2.848.2010 Salt Titrino plus
2.848.1020 Salt Titrino plus with printer
2.905.4010 Food Titrando with tiamoTM light

Water Determination according to Karl Fischer

Coulometric KF Titration
2.851.0010 851 Titrando including titration vessel, generator electrode
with diaphragm and 801 magnetic stirrer
2.851.0110 851 Titrando including titration vessel, generator electrode without diaphragm,
without 801 magnetic stirrer
2.852.0050 852 Titrando including vol. and coul. titration vessel, generator electrode with
diaphragm and 801 magnetic stirrer
2.852.0150 852 Titrando including vol. and coul. titration vessel, generator electrode without diaphragm,
without 801 magnetic stirrer
2.801.0040 801 magnetic stirrer with titration stand

Volumetric KF Titration
2.890.0110 890 Titrando with 840 Touch Control
2.890.0210 890 Titrando with tiamoTM light
2.870.1010 870 KF Titrino plus complete
2.901.0010 901 Titrando including titration vessel and indicator electrode

KF Sample Preparation
2.860.0010 860 KF Thermoprep
2.874.0010 874 Oven Sample Processor
2.136.0100 Polytron PT 1300 D

Automation
2.862.1010 862 Food/Beverage Compact Titrosampler
2.862.1110 862 Food/Beverage Compact Titrosampler with printer
2.862.2010 862 Salt Compact Titrosampler
2.862.2110 862 Salt Compact Titrosampler with printer

2.815.1110 815 Robotic Titration Soliprep

2.815.2110 815 Robotic Flexible Soliprep
2.815.3110 815 Robotic Filtration Soliprep
2.815.4110 815 Robotic Soliprep for LC
 31

Ion Chromatography
2.850.3030 850 Professional IC AnCat – MCS for anion and cation determinations
2.881.0030 881 Compact IC pro Anion – MCS for the analysis of dairy products
2.844.0020 844 UV/VIS Compact IC with PCR for bromate determination in water samples
2.871.0010 871 Advanced Bioscan for pulsed amperometric detection of carbohydrates

2.858.0020 858 Professional Sample Processor for the automation of determinations

2.800.0010 800 Dosino for full automatic liquid handling of samples
6.5330.000 IC equipment for dialysis
6.5330.010 IC equipment for ultrafiltration
6.5330.020 IC equipment for dilution

6.6059.202 MagIC NetTM 2.0 Professional

6.1005.110 Phenomenex Star Ion A300 for bromate determination

6.1006.510 Metrosep A Supp 5 – 100 for anion determination

Oxidation Stability
2.743.0014 743 Rancimat for oils and fats (230 V) including software and accessories
2.743.0015 743 Rancimat for oils and fats (115 V) including software and accessories

Voltammetry
2.797.0010 797 VA Computrace for trace analysis (manual operation)
MVA-2 797 VA Computrace system for trace analysis with automatic standard addition (consisting of
797 VA Computrace with two 800 Dosinos for automatic addition of auxiliary solutions)
MVA-3 Fully automated 797 VA Computrace system for trace analysis (consisting of
797 VA Computrace with 863 Compact VA Autosampler and two 800 Dosinos for automatic
addition of auxiliary solutions; automatic processing of up to 18 samples)

Process Analysis
2.875.0010 875 ProcessLab Base Unit with TFT operating panel, left-hinged door
2.875.0020 875 ProcessLab Base Unit with TFT operating panel, right-hinged door
2.875.0510 875 ProcessLab Base Unit with TFT operating panel including touch function, left-hinged door
2.875.0520 875 ProcessLab Base Unit with TFT operating panel including touch function, right-hinged door
2.875.0210 875 ProcessLab Base Unit VA with TFT operating panel including touch function, right-hinged door
Subject to change without prior notice
Layout by Ecknauer+Schoch ASW; printed by Metrohm AG, 9101 Herisau, Switzerland
8.000.5023EN – 2009-11

food.metrohm.com