Sampling Techniques of

UNIT 11 SAMPLING TECHNIQUES OF Food Products

FOOD PRODUCTS
Structure
11.0 Objectives
11.1 Introduction
11.2 Sample Collection
11.2.1 Homogenous Versus Heterogeneous Populations
11.2.2 Manual Versus Continuous Sampling
11.2.3 Importance of Sample Collection
11.2.4 Errors in Analytical Results due to Improper Sampling
11.2.5 Risks Associated with Sampling
11.3 Sampling Standards
11.4 The Sampling Plan
11.4.1 Understanding a Sample Plan
11.4.2 Statistical Approaches
11.5 Sampling Techniques/Methods
11.5.1 Probability Sampling
11.5.2 Non-probability Sampling
11.5.3 Types of Sampling
11.5.4 Operating Characteristic (OC) Curves
11.5.5 Requirements of Good Sampling Methods
11.5.6 Cost of Sampling
11.5.7 Problems in Sampling
11.6 Three Class Sampling Plan
11.7 Preparation of Sampling Plans
11.7.1 Model Sampling Plan
11.8 Sub Sampling for Analysis and Taking the Test Portion
11.8.1 Composite Lab Sample Preparation
11.8.2 Opinions of Experts
11.9 Sample Preparation for Analysis
11.9.1 Precautions to be Followed while Preparing a Sample for Analysis
11.10 Difficulties in Sampling
11.10.1 Example for Effect of Sampling on Analytical Result
11.11 Sample Accountability
11.11.1 Documentation
11.11.2 Chain of Custody Form
11.11.3 Sample Receipt and Handling
11.11.4 Monitoring of Samples
11.12 Retention of Samples and Records
11.12.1 Identify the Properties of Retained Samples
11.12.2 Retention Period
11.13 Case Study
11.14 Let Us Sum Up
11.15 Key Words
11.16 Answers to Check Your Progress Exercises
11.17 Some Useful Books

11.0 OBJECTIVES
After reading this unit, we shall be able to:
• state the importance of sampling in analysis of food products;
• enlist standards and guides on sampling;
• prepare sampling plans;
• describe different sampling techniques; and
• devise ways to draw a representative sample from lots.
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Food Analysis
11.1 INTRODUCTION
To control food quality and acceptance within satisfactory limits, it is
important to monitor the vital characteristics of raw materials, ingredients, and
processed foods. This could be done by evaluating all foods or ingredients
from a particular lot, which is feasible if the analytical technique is rapid and
non-destructive. However, it is usually more practical to select a portion of the
total product volume and assume the quality of the selected portion is typical
of the whole lot.
Obtaining a portion, or sample, that is representative of the whole is referred to
as sampling, and the total quantity from which a sample is obtained is called
the population. Adequate sampling technique helps to ensure that sample
quality measurements are an accurate and precise estimate of the quantity of
the population. By sampling only a fraction of the population, a quality
estimate can be obtained more quickly and with less expense and personnel
time than if the total population were measured. The sample is only an estimate
of the value of the population, but with proper sampling technique, it can be a
very accurate estimate.

11.2 SAMPLE COLLECTION

It is important to clearly define the population that is to be sampled. The
population may vary in size from a production lot, a day's production, to the
contents of a warehouse. Extrapolating information obtained from a sample of
a production lot to the population of the lot can be done accurately, but
conclusions cannot be drawn from data describing larger populations, such as
the whole warehouse.
Populations may be finite, such as the size of a lot, or infinite, such as in the
number of temperature observations made of a lot over time. For finite pop-
ulations, sampling provides an estimate of lot quality. In contrast, sampling
from infinite populations provides information about a process. Fig.11.1
represents the sampling for physical and chemical characteristics of food.
Regardless of the population type, that is, finite or infinite, the data obtained
from sampling are compared to a range of acceptable values to ensure the
population sampled is within specifications.
11.2.1 Homogeneous Versus Heterogeneous Populations
The ideal population would be uniform throughout and identical at all
locations. Such a population would be homogeneous. Sampling from such a
population is simple, as a sample can be taken from any location and the
analytical data obtained will be representative of the whole. However, this
occurs rarely, as even in an apparently uniform product, such as sugar syrup,
suspended particles and sediments in a few places may render the population
heterogeneous. In fact, most populations that are sampled are heterogeneous.
Therefore, the location within a population where a sample is taken will affect
the subsequent data obtained. However, sampling plans and sample preparation
can make the sample representative of the population or take heterogeneity into
account in some other way.
11.2.2 Manual Versus Continuous Sampling
To obtain a manual sample the person taking the sample must attempt to take a
"random sample" to avoid human bias in the sampling method. Thus, the

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sample must be taken from a number of locations within the population to Sampling Techniques of
ensure it is representative of the whole population. For liquids in small Food Products
containers, this can be done by shaking prior to sampling. When sampling
from a large volume of liquid, such as that stored in silos, aeration ensures a
homogeneous unit. Liquids may be sampled by pipetting, pumping, or dipping.
However, when sampling grain from a rail car, mixing is impossible and
samples are obtained by probing from several points at random within the rail
car. Such manual sampling of granular or powdered material is usually
achieved with triers or probes that are inserted into the population at several
locations. Errors may occur in sampling, as rounded particles may flow into
the sampling compartments more easily than angular ones. Similarly,
hygroscopic materials flow more readily into the sampling devices than does
non hygroscopic material. Horizontal core samples have been found to contain
a larger proportion of smaller-sized particles than vertical ones. Continuous
sampling is performed mechanically.
Qualitative Characteristics
(e.g. commodity defects )

Inspection of isolated lots. Inspection of a continuous series of lots.

E.g., inspection of the aspects of a piece of fruit, E.g., inspection of the aspects of a piece of fruit,
or of a can in isolated lots. or of a can in continuous lots.

To be sampled by attribute sampling plan for To be sampled by attribute sampling plans for
isolated lots. continuous lots.

Quantitative characteristics
(e.g., compositional characteristics)

Inspection of isolated lots Inspection of continuous series of lots

Bulk Item Bulk Item

e.g. fat content of e.g. sodium e.g.: fat content e.g. sodium
milk in a tank content of a of milk in a tank. content of a
dietary cheese. dietary cheese.

To be sample by Sampling by To be sampled To be sampled

variable sampling attributes. by variable by attribute
plans for sampling plans sampling plans
isolated lots for continuous for continuous
series of lots. series of lots.

Fig. 11.1: Sampling Flowchart for Chemical and Physical Characteristics

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Food Analysis 11.2.3 Importance of Sample Collection
The reliability of analytical data thus obtained depends on several factors,
sampling being the major factor. Current analytical methods require only few
grams of food sample to analyze. Thus, it is necessary that a sample be as
representative of the population as possible.
There are three basic activities involved in analysis of food products:
• Collection of representative sample.
• Sample preparation.
• Analysis using appropriate methods and instruments.
These activities, although independent in nature, yet can have decisive
influence on each other. Furthermore, each of these activities have their own
potential sources of variations that contribute to the uncertainty level
associated with any analytical result. Thus, care must be taken to identify the
sources of variation and minimize or avoid them while accomplishing any
activity. On the part of the laboratories, it is therefore necessary to develop a
plan for the proper performance of each activity, and then establish quality
standards and written procedures in compliance with the standards. Many
times, the activity of sampling falls outside the purview of a laboratory’s
mandate or control. This is especially true in commercial testing laboratories
where the “first contact” is the arrival of samples. To improve the overall
quality of the analytical process, a laboratory must do all it can to receive
appropriate, applicable, defensible samples. The development of appropriate
plans will depend upon an understanding of the problems involved in each
activity, and then the application of reasonable judgements in seeking
solutions.
It should be noted that sampling terminology and procedures used may vary
between companies and between specific applications. However, the principles
described in this Unit are intended to provide a basis for understanding,
developing, and evaluating sampling plans and sample handling procedures for
specific applications encountered.
A sample should represent a population as adequately as possible. To ensure
proper sampling, the analysts need to be consulted time to time concerning
proper sample size, suitable containers for sampling or the use of appropriate
preservatives to prevent any spoilage or transformation in a sample before
analysis. One common cause of lack of precision or lab-to-lab variation in
analytical results for a particular population can be traced back to erroneous
sampling. For example, in case of grapes, a laboratory sample size of meager
3 kg berries represents the whole population of > 10000 kg in 1 hectare
vineyard area. Thus, if the sample collected is not representative, then there
will be sample-to-sample variation in results. When significant difference in
results occurs among laboratories which have supposedly analyzed the same
sample, a serious conflict may arise questioning the competence and credibility
of the laboratories. Many of these situations can be avoided if samples are
collected according to a rational plan that gives some assurance that the sample
delivered to the laboratory represents the composition of the parent lot.
There are at least two ways to measure a given lot of goods: one, that we often
assume to be the “proper” way, is to find its “true value”, by which we mean
its average value. The other way, often discovered accidentally as a result of
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“poor” sampling, is to measure its variability. So called proper sampling of Sampling Techniques of
drug dosage forms, for example, may involve compositing 20 tablets, by which Food Products
the majority of the tablets could be used to dilute and conceal the fact that
several of them are severely sub- or super- potent. Similarly, two lots of grain
may have been purposely, but ineffectively, mixed in an attempt to reduce the
average level of a contaminant. Sampling that led to the laboratory finding
inconsistent results would reveal the attempt to dilute an illegal product.

11.2.4 Errors in Analytical Results due to Improper Sampling

Few studies have been conducted on the distribution of error among the three
activities: sampling, sample preparation, and analysis. In one such study,
which involved analysis of 20 nanogram/gram concentration of aflatoxin in a
lot of peanuts, the error contributed by the sampling step was as high as 67%
of the total variance, in comparison to 20% and 13% errors contributed by the
analyst and the analytical procedure, respectively. In a field study conducted
at the National Research Centre for Grapes, Pune, the pesticide residues in
grape samples analyzed in 15 individual grape bunches collected out of 1 acre
area showed above 50% sampling-induced variations. The results of such
experimentations are not unusual and it illustrates the proportion of error that
can be attributed to sampling. For peanuts, the distribution of aflatoxin can
vary widely, with a few peanuts accounting for most of the contamination.
Similarly, in case of the field sampling of grapes, the pesticide residues might
have deposited in variable concentrations in different grape bunches and thus
when they were analyzed separately, showed variable results. The important
point in these examples is to show that sampling error can play a very
significant part in the overall error in the analytical system.

11.2.5 Risks Associated with Sampling

There are two types of risks associated with sampling. Both should be
considered when developing a sampling plan. The consumer risk describes the
probability of accepting a poor quality population. This should happen rarely
(<5% of the lots) but the actual acceptable probability of a consumer risk
depends on the consequences associated with accepting an unacceptable lot.
These may vary from major health hazards and subsequent fatalities to a lot
being of slightly lower quality than standard lots. Obviously, the former
demands a low or no probability of occurring whereas the latter would be
allowed to occur more frequently. The second risk i.e., vendor risk is the
probability of rejecting an acceptable product. As with consumer risk, the
consequences of an error determine the acceptable probability of the risk. An
acceptable probability of vendor risk is usually 5-10%.

11.3 SAMPLING STANDARDS

Data obtained from an analytical technique are the result of a stepwise
procedure from sampling, to sample preparation, laboratory analysis, data
processing, and data interpretation. There is a potential for error at each step
and the uncertainty, or reliability, of the final result depends on the cumulative
errors at each stage. Variance is an estimate of the uncertainty. The total
variance of the whole testing procedure is equal to the sum of the variances
associated with each step of the sampling procedure and represents the
precision of the process. Precision is a measure of the reproducibility of the
data. In contrast, accuracy is a measure of how close the data are to the true
value. The most efficient way to improve accuracy is to improve the reliability
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Food Analysis of the step with the greatest variance. Frequently, this is the initial sampling
step. The reliability of sampling is dependent more on the sample size than on
the population size. The larger the sample size, the more reliable the sampling.
However, sample size is limited by time, cost, sampling methods, and the
logistics of sample handling, analysis, and data processing.
It should be noted that sampling terminology and procedures used may vary
between companies and between specific applications. Several standards and
recommendations provide the ways and means to sample a particular lot.
ISO specifies various standards and guidelines for drawing samples and data
interpretation for samples. Few such standards related to food are mentioned in
Table 11.1.
Table 11.1: Standards and Guides of Sampling

ID of Standard/Guide Title of Standard/Guide

ISO 2854 : 1976 Statistical Interpretation of data- techniques of estimation and

tests relating to means and variances.

ISO 2859-0 : 1995 Sampling procedures for inspection by attributes-Part 0 ;

Introduction to the ISO 2859 Attribute sampling system

ISO 2859-1 : 1999 / Sampling procedures for inspection by attributes-Part 1;

Sampling plans indexed by Acceptable Quality Level (AQL) for
IS 2500 (Part I) : 1989 lot-by-lot inspection.

IS 2500 (Part II) : 1965 Sampling inspection procedures.

ISO 2859-2 : 1985 Sampling procedures for inspection by attributes- Part 2;

Sampling plans indexed by Limiting Quality (LQ) for isolated lot
inspection.

ISO 3494 : 1976 Statistical interpretation of data – Power of tests relating to mans
and variances.

ISO 3951 : 1989 Sampling procedures and charts for inspection by variables for
per cent non-conforming.

ISO 5725-1 : 1994 Application of statistics- Accuracy (trueness and precision) of

measurement methods and results- Part 1; General principles and
definitions.

ISO 7002 : 1986 Agricultural food products-Layout for a standard method of

sampling a lot.

ISO 8423 : 1991 Sequential sampling plans for inspection by variables for per cent
non-conforming (known standard deviation).

ISO 8422 : 1991 Sequential sampling plans for inspection by attributes.

ISO/ TR 8550 : 1994 Guide for the selection of an acceptance sampling system,
scheme or plan for inspection of discrete items in lots.

ISO 10725 : 2000 Acceptance sampling plans and procedures for the inspection of
bulk material.

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 Sampling Techniques of
ISO/ FDIS 11648/1 Statistical aspects of sampling from bulk materials – Part 1; Food Products
General principles.

ISO/ DIS 14560 Acceptance sampling procedures by attributes – specified quality

levels in non-conforming items per million.

Other IS specifications Specifications published by BIS pertaining to individual products

contain the details of lot size and corresponding number and
quantity of samples to be drawn and tested for conformance.

Since all standards are subject to revision, parties to agreements based up on

these guidelines should ensure that the most recent editions of the standards
are always applied.
An example for flour sampling as per AOAC method is presented here. The
AOAC Method 925.08 (6) describes the method for sampling flour from
sacks. The number of sacks to be sampled is determined by the square root of
the number of sacks in the lot. The sacks to be sampled are chosen according
to their exposure. The samples that are more frequently exposed are sampled
more often than samples that are exposed less. Sampling is done by drawing a
core from a corner at the top of the sack diagonally to the center. The sampling
instrument is a cylindrical, polished trier with a pointed end. It is 13 mm in
diameter with a slit at least one third of the circumference of the trier. A
second sample is taken from the opposite corner in a similar manner. The
cores are stored for analysis in a clean, dry, airtight container that has been
opened near the lot to be sampled. The container should be sealed immediately
after the sample is added. A separate container is used for each sack.
Additional details regarding the container and the procedure also are described
below.
Title 21 CFR specifies the sampling procedures required to ensure that specific
foods conform to the standard of identity. In the case of canned fruits, 21 CFR
145.3 defines a sample unit as "container, a portion of the contents of the
container, or a composite mixture of product from small containers that is
sufficient for the testing of a single unit". Furthermore, a sampling plan is
specified for containers of specific net weights. The container size is
determined by the size of the lot. A specific number of containers must be
filled for sampling of each lot size. The lot is rejected if the number of
defective units exceeds the acceptable limit. For example, out of a lot
containing 48,001 to 84,000 units, each weighing 1 kg or less, 48 samples
should be selected. If six or more of these units fail to conform to the attribute
of interest the lot will be rejected. Based on statistical confidence intervals,
this sampling plan will reject 95% of the defective lots examined, that is, 5%
consumer risk.
Table 11.2: Minimum Number of Primary Samples to be taken from a Lot
(Ref: CODEX doc. CAC/GL 33)

Name of Commodity Minimum Number of Primary Samples to be taken

from a Lot

1. Meat and Poultry

a) Non-suspect lot 1

b) Suspect lot Determined according to Table 11.3

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Food Analysis 2. Other products

a) Products packaged in bulk, 1

which can be assumed to be
(A lot may be mixed by grading or manufacturing
well mixed or homogeneous.
process)

b) Products packaged in bulk, For products comprised of large units, the minimum
which may not be well mixed number of primary samples should comply with the
or homogeneous. minimum number of units required for the laboratory
sample.

Either Weight of lot, kg

<50 3

50-500 5

>500 10

or, Number of cans, cartons,

containers in the lot

1-25 1

26-100 5

> 100 10

Table 11.3: Number of randomly selected primary samples required for a given
probability of finding at least one non-compliant sample in a lot of meat or
poultry for a given incidence of non-compliant residue in the lot
(Ref: CODEX doc. CAC/GL 33)

Incidence of Non- Minimum number of samples (no ) required to detect a

compliant non- compliant residue with a probability of
Residues in the Lot
% 90% 95% 99%
90 1 - 2
80 - 2 3
70 2 3 4
60 3 4 5
50 4 5 7
40 5 6 9
35 6 7 11
30 7 9 13
25 9 11 17
20 11 14 21
15 15 19 29
10 22 29 44
5 45 59 90
1 231 299 459
0.5 460 598 919
0.1 2302 2995 4603

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Notes: Sampling Techniques of
Food Products
a) The table assumes random sampling.
b) Where the number of primary samples indicated in Table 11.2 is more than about
10% of units in the total lot, the number of primary samples taken may be fewer
and should be calculated as follows:
no
n=
1 + (no-1 ) / N
Where, n = minimum number of primary samples to be taken
no = number of primary samples given in Table 11.2
N = number of units, capable of yielding a primary sample in the lot.
c) Where a single primary sample is taken, the probability of detecting a non-
compliance is similar to the incidence of non-compliant residues.
d) For exact or alternative probabilities, or for a different incidence of non-
compliance, the number of samples to be taken may be calculated from:
1 – p = ( 1 – i )n
Where, p is the probability and i is the incidence of non-compliant residue in the lot
(both expressed as functions, not percentages) and n is the number of samples.
Table 11.4: Sampling Procedure and Minimum Amount (composite/bulk) to be Sampled
from lots

Crop Type Sampling Procedure Example Minimum

Quantity
Root, tuber Take samples from all areas Beet (red, sugar, fodder), 5 kg
and bulb of the crop. Remove as onions, parsnips, potatoes, (and not less
vegetables much adhering soil as sweet potatoes, turnips than 5 items)
possible from samples but
do not wash.
(Note: In some cases, where Carrots, radish, spring 2 kg
leaf parts are used as stock onions.
feed, they may need to be
sampled separately).
Take the sample from all Brassica (cabbage, 5 kg
areas of the crop. Sample cauliflower, broccoli, (and not less
parts of the crop exposed to kohlrabi, curly kale). than 5 items)
the spray and also those
apparently protected by
foliage.
Leafy, stem, Remove as much soil as Asparagus, brussel 2 kg
fruiting and possible from crops such as sprouts, celery, chicory,
legume celery, but do not wash. lettuce, spinach, turnip
vegetables tops
Cucumber, melon, 5 kg
squashes, eggplant (and not less
than 5 items)
Peppers, tomatoes, 2 kg
gherkins
Beans, peas, etc. (with 2 kg
pods)
All tree and Select fruit from all parts of Apples, citrus, peaches, 5 kg
bush fruit, the tree/bush, high and low, pears
including and from both sides of the
vines, small row, and select fruits
fruits and according to abundance
berries whether in each segment or
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Food Analysis the whole tree/bush. More
fruit should therefore be
selected from the more
densely laden parts of the
crop.
Sample parts of the crop Cherries, nuts, olives, 2 kg
exposed to the spray and plums.
also those apparently
protected by foliage.
Take large and small fruits, Bush fruit (all types), 2 kg
perfect or slightly grapes, strawberries
blemished, but not so small
or blemished that they
would not normally be
saleable.
Cereal Cut not less than ten small Maize (grain and cobs) 2 kg
Grains areas (approximately 0.1 m2)
chosen randomly from all
areas of the crop. Cut stalks
about 10 cm above the
ground. Remove grain from
the straw.
Oil Seeds Collect the heads when they Sesame, canola, 1 kg of seeds
have reached the stage of soybeans, sunflower
maturity at which they are
normally harvested and if
convenient thresh to remove
the seeds.

Table 11.5: Description of Primary samples and min. size of laboratory sample
(Ref: CODEX doc. CAC/GL 33)
S. No Commodity Examples Nature of Primary Minimum Size of
Classification Samples to be taken Lab Sample
1. Primary food commodities of animal origin
1.1 Large mammals Cattle Whole or part of 0.5 kg
Whole or half carcass Sheep diaphragm,
supplemented by
Usually 10 kg or more Pigs cervical muscles, if
Necessary

1.2 Small mammals Rabbits Whole carcass or hind 0.5 kg, after
Whole carcass quarters removal of skin
and bone

1.3 Mammal meat parts, Quarters Whole unit(s),or a 0.5 kg, after
loose Chops portion of a large unit removal of bone
fresh/chilled/frozen
Steaks
Packaged or other wise
Shoulders
1.4 Mammal meat parts, Quarters Either a frozen cross- 0.5 kg, after
bulk frozen Chops section of a container removal of bone
or the whole (or
portions of individual)
meat parts
2. Poultry fats
2.1 Birds, at slaughter Chickens Units abdominal fat 0.5 kg
whole or part-carcass Turkeys from at least three birds

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2.2 Bird meat parts Legs Either visible fat, 0.5 kg Sampling Techniques of
Breast – trimmed from units Food Products
muscle
Whole units or portions 2 kg
where fat is not
trimmable
2.3 Bird fat tissue in bulk Units taken with a 0.5 kg
sampling device from
at least three portions
2.4 Poultry eggs Whole eggs 12 whole eggs

2.5 Liquid, frozen or dried Whole units 0.5 kg

egg products
3. Processed foods of animal origin
3.1 Mammal or bird Ham Packaged units or a 0.5 kg or 2 kg if
comminuted, cooked, sausage / representative cross fat content
canned, dried, rendered Minced section from a < 5%
or otherwise processed beef / container or units
products including multi (including juices, if
ingredient products Chicken any) taken with a
paste sampling device
3.2 Liquid milks, milk Packaged units 0.5 L or
powders, ice creams etc. 0.5 kg
3.3 Cheese Units > Whole unit 0.5 kg
0.3 kg
Units < Whole unit 0.3 kg
0.3 kg
4. Herbs Fresh Whole units 0.5 kg
Dried Whole units 0.1 kg
5. Feed commodities of plant origin
5.1 Legume animal Whole units 1 kg (at least 10
feeds and other units)
forages and fodders
5.2 Straw, hay and Units taken with a 0.5 kg (at least
other dry products sampling device 10 units)
6. Processed foods of plant origin
6.1 Products of high Packages or units 0.1 kg
unit value taken with a
sampling device
6.2 Solid products of Hops Packages or units 0.2 kg
low bulk density Tea taken with a
sampling device
6.3 Other solid Bread Packages or units 0.5 kg
products Flour taken with a
Dried fruits sampling device
Vegetable
6.4 Liquid products Oils Packages or units 0.5 L or
Juices taken with a 0.5 kg
sampling device

"
Check Your Progress Exercise 1
Note: a) Use the space below for your answers.
b) Check your answers with those given at the end of the unit.
15
Food Analysis 1) What is the importance of sample collection in analysis of food products?
………………………………………………………………………………
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2) What are homogenous and heterogeneous populations?
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11.4 THE SAMPLING PLAN

11.4.1 Understanding a Sample Plan
Sampling is generally done for a specific purpose and the purpose may indeed
suggest or dictate the nature of any sampling plan. The International Union of
Pure and Applied Chemistry (IUPAC) defines a sampling plan as "a
predetermined procedure for the selection, withdrawal, preservation,
transportation, and preparation of the portions to be removed from a lot as
samples". A sampling plan should be a well-organized document that
establishes the required procedures for accomplishing the program's objectives.
It should address the issues of who, what, where, why, and how. The primary
aim of sampling is to obtain a sample, subject to constraints on size, that will
satisfy the sampling plan specifications. A sampling plan should be selected on
the basis of the sampling objective, the study population, the statistical unit, the
sample selection criteria, and the analysis procedures. Factors determing the
choice of a sampling plan are enlisted in Table 11.6. The two primary
objectives of sampling are often to estimate the average value of a
characteristic and determine if the average value meets the specifications
defined in the sampling plan. The presence of a well designed plan is important
because it provides a consistent model to guide people performing the
sampling activity, and it serves as a reminder of the important elements in this
part of the overall sample analysis program.
Table 11.6: Factors Affecting Choice of Sampling Plans

Factors to be considered Questions

Purpose of inspection a Is it to accept or reject the lot?
b Is it to measure the average quality of the lot?
c Is it to determine the variability of the product?
Nature of Product a Is it homogeneous or heterogeneous?
b What is the unit size?
c How consistently have past populations met specifications?
d What is the cost of the material being sampled?
Nature of the test method a Is the test critical or minor?
b Will someone become sick or die if the population fails to
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 pass the test? Sampling Techniques of
c Is the test destructive or non-destructive? Food Products

d How much does the test cost to complete?

Nature of the population a Is the lot large but uniform?
being investigated b Does the lot consist of smaller, easily identifiable sublots?
c What is the distribution of the units within the population?

11.4.2 Statistical Approaches

In many sampling programs, statistical approaches are not given the requisite
attention. Percentage sampling systems that specify a fixed percentage of a lot,
say 5 or 10%, do not provide the quality protection that is often assumed.
Statistical sampling theory furnishes the means to analyze the relationship
between a lot of goods and the samples that are drawn from it. It can be used
to estimate population measure, or “parameters,” such as variance and
correlation, from knowledge of corresponding samples quantities. The
importance of sampling is recognized in ISO 17025, (this standard will be
discussed in detail in Course 5, Block 3) which requires that test reports make
reference to the sampling procedure used by the laboratory or the submitting
body.

Check Your Progress Exercise 2

"
Note: a) Use the space below for your answers.
b) Check your answers with those given at the end of the unit.
1) Sampling plan is very important in sampling. Why?
………………………………………………………………………………
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2) Mention the purposes that are served by a sampling plan.
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11.5 SAMPLING TECHNIQUES/METHODS

There are several sampling methods/techniques in common use. These are
probability sampling, non-probability sampling, bulk sampling, and acceptance
sampling. These are described in brief below:

11.5.1 Probability Sampling

Probability sampling is used when a representative sample is desired, and uses
principles of statistical sampling and probability i.e. elimination of human bias.

17
Food Analysis It is a random selection approach that tends to give each unit an equal chance
of being selected.
Simple random sampling requires that the number of units in the population
be known and each unit is assigned a number. A specific quantity of random
numbers between one and total number of population units is selected. Sample
size is determined by lot size and potential impact of a consumer or vendor
error. Units corresponding to the random numbers are then analyzed as an
estimate of the population.
Systematic sampling is used when a complete list of sample units is not
available, but when samples are distributed evenly over time or space, such as
on a production line. The first sample is selected at random and then every nth
unit after that.
Stratified sampling involves dividing the population into overlapping
subgroups so that each subgroup is as homogenous as possible. Group means,
therefore, differ from each other as much as possible. Random samples are
then taken from each subgroup. The procedure provides a representative
sample because no part of the population is excluded and it is less expensive
than simple random sampling.
Cluster sampling entails dividing the population into clusters or subgroups so
that cluster’s characteristics are as identical as possible, that is, the means are
very similar to each other. Any heterogeneity occurs within each cluster.
Clusters should be small and having a similar number of units in each cluster.
The clusters are sampled randomly and may be either totally inspected or sub-
sampled for analysis. This sampling method is more efficient and less
expensive than simple random sampling, if populations can be divided into
homogenous groups.
Composite sampling is used to obtain samples from bagged products such as
flour, seeds, and larger items in bulk. Two or more samples are combined to
obtain one sample for analysis that reduces differences between samples. For
example, FDA composite 12 and at least six subsamples, respectively, for the
sample to be analyzed for compliance with nutrition labeling regulations.

11.5.2 Non-probability Sampling

Non-probability sampling is used when it is not possible to collect a
representative sample, or a representative sample is not desired. For example,
in case of adulteration such as rodent contamination, the objective of the
sampling plan may be to highlight the adulteration rather than collect a
representative sample of the population. The sample collector uses judgement
rather than statistical considerations in the selection of the sample. The unusual
or unexpected characteristics in a population could be selected to be identified.
This type of sampling is done in many ways, but in each case the probability of
including any specific portion of the population is not equal because the
investigator selects the samples without estimating sampling error.
Judgement sampling is solely at the discretion of the sampler and therefore is
highly dependent on the person taking the sample. This method is used when it
is the only practical way of obtaining the sample. This method may present a
better estimate of the population than random sampling if sampling is done by
an experienced individual and limitations of extrapolations from the results are
understood.
18
Convenience sampling is performed when ease of sampling is the key factor. Sampling Techniques of
The first pallet in a lot or the sample that is most accessible is selected. This Food Products
type of sampling will not be representative of the population, and therefore is
not recommended.
Restricted sampling may be unavoidable when the entire population is not
accessible. For example, if sample is to be taken from a loaded truck, but the
sample is not a representative of the entire population.
Quota sampling is the division of a lot into groups representing various
categories, and samples are then taken from each group. This method is less
expensive than random sampling but also is less reliable.

11.5.3 Types of Sampling

A) Bulk sampling
Bulk sampling involves the selection of a sample from a lot of material that
does not consist of discrete, identifiable or constant units. Sampling may be
performed in static or dynamic situations. Bulk sampling poses special
problems requiring certain decisions to be made: the number of increments to
be taken, the size of the increments, from where in the pile or stream they
should be drawn, the sampling device to be used, and how to reduce the
increments taken to a reasonable size of sample for delivery to the laboratory.
B) Acceptance sampling
Acceptance sampling differs from the previous types and involves the
application of a predetermined plan to decide whether a lot of goods meet
defined criteria for acceptance. The risks of accepting “bad” or rejecting
“good” lots are stated in conjunction with one or more parameters, for
example, quality indices of the plan. Statistical plans can be designed to
regulate the probabilities of rejecting good lots or accepting bad lots.
Refer Tables 11.2 and 11.3 in the annexure.
There are two broad categories of acceptance sampling: sampling by attributes
and sampling by variables.
Sampling by attributes
In sampling by attributes, the unit of product is classified as defective or non-
defective, or the number of defects in a unit of product is counted with respect
to a given requirement. Or, the sampling is performed to decide on the
acceptability of a population based on whether the sample possesses a certain
characteristic, for example, Clostridium botulinum contamination in canned
goods. An example of net weight determination may serve to explain the
differences between the two categories. In attribute sampling, each unit that
weighs 1 pound or more is accepted, and each unit that weighs less than 1
pound is rejected. If the number of rejects exceeds a predetermined number,
the lot is rejected. If the number of rejects is less than the predetermined
number, the lot is accepted.
Sampling by variables
In variable sampling, sampling is performed to estimate quantitatively the
amount of a substance (e.g., salt) or a characteristic (e.g., color) on a contin-
uous scale. The estimate obtained from the sample is compared with an
19
Food Analysis acceptable value (i.e., previously determined) and the deviation measured. This
type of sampling usually produces data that have a normal distribution such as
in the per cent fill of a container and total solids of a food sample. In general,
variable sampling requires smaller sample size than attribute sampling and
each characteristic should be sampled for separately when possible.

11.5.4 Operating Characteristic (OC) Curves

Operating Characteristic (OC) curves are used extensively in acceptance
sampling. The OC curve shows the relationship between the quality and the per
cent of lots expected to be acceptable for the quality characteristic inspected.
In other words, the OC curve is a graph of lot defectives against the probability
that the sampling plan will accept the lot. Fig. 11.2 depicts OC curves for an
ideal sampling plan.

Fig. 11.2: Operating Characteristic Curve

The Operating Characteristic (OC) curve shows the probability of acceptance,

Pa, for any level of lot quality. On the horizontal axis is the quality
characteristic. This OC curve enables you to evaluate the probability of
acceptance for any true lot quality level-on a what-if basis. This way, you can
design sampling plans that perform the way you want.
We can interpret the curve according to this example:
1) If the lot quality is 0.093 fraction defective, then the probability of
acceptance, Pa, is 0.05.
2) If the lot quality is 0.018 fraction defective, then the probability of
acceptance, Pa, is 0.95.

11.5.5 Requirements of Good Sampling Methods

Samples are useful for their intended purpose when they are taken in a manner
consistent with generally recognized good sampling techniques and good
sampling practices. This requires the following:
• Inspection of the lot before sampling.
• Use of suitable sampling devices for the particular commodity and type of
sample desired.
• Use of suitable containers to hold the sample.
• Maintenance of the integrity of the sample and associated records.
• Use of adequate precautions in preserving, packing and delivery of the
sample to the lab in a timely manner.
20
• Provision of appropriate storage conditions for the sample both prior to and Sampling Techniques of
following analysis. Food Products

All of these factors, along with others such as cost versus benefits analysis, and
a review of program objectives and regularity requirements, are to be assessed
and brought together in a sampling plan that serves as a guide to management,
as well as to operating personnel as a firm plan to achieve quality in sampling.

11.5.6 Cost of Sampling

The attention of users is drawn upon relation between the efficiency and size of
sample. For a given Acceptable Quality Level (AQL), the smaller the sample
size, the smaller the cost of sampling, but the worse the efficiency, that is the
risk to wrongly accepting a lot increases and worsens the damage in trade.

11.5.7 Problems in Sampling

Analytical data never are more reliable than the sampling technique. Sampling
bias, due to non-statistically viable convenience, may compromise reliability.
Errors also may be introduced by not understanding the population distribution
and subsequent selection of an inappropriate sampling plan.
Unreliable data also can be obtained by non-statistical factors such as poor
sample storage resulting in sample degradation. Samples should be stored in a
container that protects the sample from moisture and other environmental
factors that may affect the sample (e.g., heat, light, air). To protect against
changes in moisture content, samples should be stored in an airtight container.
Light sensitive samples should be stored in containers made of opaque glass, or
the container wrapped in aluminum foil. Oxygen sensitive samples should be
stored under nitrogen or an inert gas. Refrigeration or freezing may be
necessary to protect chemically unstable samples. However, freezing should be
avoided when storing unstable emulsions. Preservatives (e.g., mercuric
chloride, potassium dichromate, and chloroform) can be used to stabilize
certain food substances during storage.
Mislabeling of samples causes mistaken sample identification. Samples should
be clearly identified by markings on the sample container in a manner such that
markings will not be removed or damaged during storage and transport. For
example, plastic bags that are to be stored in ice water should be marked with
water-insoluble ink.
If the sample is an official or legal sample the container must be sealed to
protect against tampering and the seal mark easily identified. Official samples
also must include the date of sampling with the name and signature of the
sampling agent. The chain of custody of such samples must be identified
clearly.

11.6 THREE CLASS SAMPLING PLAN

Another type of sampling used frequently by regulatory agencies to determine
acceptance or rejection of a lot (often defined as the quality of product
produced under essentially the same conditions but representing no more than
one day’s production) is the three-class sampling plan. This approach is often
used when assessing microbiological contamination of foods. In this case, “n”
is the number of samples, usually selected at random from the lot, the
21
Food Analysis numerical value “m“ represents acceptable concentrations, the numerical value
“M” represents un-acceptable concentrations, and “c” is the maximum
allowable number of marginally acceptable sample units such that if this
number is exceeded, the lot is considered as un-acceptable. While “m”
separates sample units of acceptable quality from those of marginally
acceptable quality, “M” separates sample units of marginally acceptable
quality from those of defective quality.
For enforcement purposes, the sampling technique used should be the same as
the sampling technique used to set the standard. For example, minimum
reportable limits for particles are based on composite samples and not on
individual lots.

11.7 PREPARATION OF SAMPLING PLANS

The development of quality sampling plans is a science in itself and has been
given consideration by a number of organizations. One plan format that
deserves serious consideration, developed by the International Organization for
Standardization, is shown with comments in ISO/TC 34, ISO/DIS 7002.2,
“Agricultural food products- Layout for a standard method of sampling from a
lot “(1988).
It can serve as a starting point or check list for developing a sampling plan for
most commodities. The title and headings from sections in the monograph are
as below:

11.7.1 Model Sampling Plan

Agricultural food products- Layout for a standard method of sampling from
a lot.
1) Title (short but appropriate for index identification)
2) Introduction (describing the purpose of the plan)
3) Scope (describing the breadth of coverage of the plan)
4) Field of application (products to be covered; where sampling will be done)
5) References (documents, the validity of the plan with reference to other
requirements)
6) Definitions (specific terms associate with a particular matrix)
7) Principle (statistical basis of the method of sampling)
8) Administrative arrangements
a) Sampling personnel
b) Representation of parties concerned
c) Health, safety and security precautions
d) Preparation of the sampling report
9) Identification and inspection of the lot prior to sampling (important in
survey sampling for identification, condition of the lot and selection of
method of sampling).
10) Sampling equipment and ambient conditions (proper tools such as use of
sterile equipment for aseptic sampling).
22
11) Sample containers and packing (essential to prevent contamination and Sampling Techniques of
damage during shipment or storage). Food Products

12) Sampling procedures (as dictated by the plan objectives).

a) Sampling size (adequate for all analytical testing to be done.
Refer Tables 11.2 to 11.4 in Annexure)
b) Taking the sample.
c) Preparation of bulk samples (Table 11.3) and reduced samples
(Table 11.4).
d) Selection of samples of pre-packaged products.
13) Packing, sealing and marking of samples and sample containers
(identification of units and to establish chain-of-custody).
a) Filling and sealing sample containers.
b) Labeling or marking (including signature of sampling personnel).
c) Packing samples for storage or transportation.
14) Precautions during storage and transportation of samples.
15) Sampling report
a) Administrative details.
b) Details of unit packs or enclosure containing the lot.
c) Material samples.
d) Marking and sealing of samples.
16) Annexure (supplemental information, if necessary).

Check Your Progress Exercise 3 "

Note: a) Use the space below for your answers.
b) Check your answers with those given at the end of the unit.
1) Mention some sampling methods/techniques related food products?
………………………………………………………………………………
………………………………………………………………………………
…………………………………………………………………………….…
……………………………………………………………………………….
………………………………………………………………………………
2) What is probability sampling?
………………………………………………………………………………
………………………………………………………………………………
………………………………………………………………………………
…………………………………………………………………………….…
………………………………………………………………………………

23
Food Analysis 3) Describe advantages and disadvantages of the plans- Sampling by
attributes and sampling by variables?
………………………………………………………………………………
………………………………………………………………………………
…………………………………………………………………………….…
……………………………………………………………………………….
4) Write down the application flow of three- class sampling plan?
………………………………………………………………………………
………………………………………………………………………………
………………………………………………………………………………
…………………………………………………………………………….…
5) Mention some basic requirements of good sampling methods?
………………………………………………………………………………
………………………………………………………………………………
………………………………………………………………………………
…………………………………………………………………………….…
6) How much quantity of sample is required for the following items?
Root and bulb vegetables, Cereal grains, Poultry eggs, Liquid milk, Liquid
products.
………………………………………………………………………………
………………………………………………………………………………
………………………………………………………………………………
…………………………………………………………………………….…

11.8 SUB SAMPLING FOR ANALYSIS AND

TAKING THE TEST PORTION
If the test portion analyzed does not represent the sample or the lot from which
it was taken, in that case, even the best analysis could give misleading
information. Distortions introduced at this point will carry through the path of
analysis and adversely affect the final results and the conclusions drawn from
them. There are generally two choices in analytical sub sampling:
• Preparation of a composite laboratory sample (if multiple units are
submitted for analysis).
• Examination of individual units.

11.8.1 Composite Lab Sample Preparation

A composite lab sample is one in which the individual units or representative
portions of units are mixed to form a uniform mixture. Portions are then taken
24
from the composite for analysis. Compositing saves analytical time and in Sampling Techniques of
some types of contract testing it may be the procedure specified. If the results Food Products
indicate that there may be a problem, it will likely be necessary to go back and
analyze individual samples. Compositing is not the procedure of choice when
there is a chance that an individual unit that constitutes a public health or
safety threats will not be detected (there are some exceptions) or where a unit
at or outside of tolerance level will not be detected because of matrix dilutions.
Multiple unit lab sampling is indicated when the possible range of values
among individual units is considered significant or it is desirable to establish
the variability of the lot.
Refer to Tables 11.4 and 11.5 for the details commodities and quantity of
sample required.

11.8.2 Opinions of Experts

You den and Steiner (Statistical Manual of the AOAC, AOAC International,
Arlington, VA, p 41) observed that, “Many materials are notoriously difficult
to sample. Often the variability among samples is the controlling factor in the
confidence placed in the analytical result.” They note further that
A mistake sometimes made is to composite several samples and then to run
repeat determinations on this composite sample. The analyst may be happy
with several results that are in close agreement because only the analytical
error is involved in the results. And some may put their faith in the result
admittedly, if the individual samples were of the same weight and properly
mixed, the same average will result whether the samples are analyzed
individually or repeats are made on the composition. Using the composite
sample effectively conceals the between-sample variation. It should be
mandatory to run the samples individually, for only by doing so will anybody
be in a position to make any statistical statements about the results, no matter
how good the analytical procedure.
Somewhat similar view of sub sampling for analysis is expressed in an article
published in Chemical and Engineering news by an ad hoc sub committee of
The American Chemical society for “Dealing with the Scientific Aspects of
Regularity Measurements.”
This report observes that the number of samples to be analyzed in a given
situation usually is limited by the resources available for collection of samples
or for their analysis. However, the reliability of the result generally increases
with the square root of the number of samples analyzed. For this reason,
analysis of multiple samples are preferred over single samples since, single
samples give no information on the homogeneity of the lot that was sampled. In
addition, for single samples, the sampling error is also confounded with the
analytical error. As a result, if the total number of determinations must be
fixed, multiple independent single samples are preferred over replicate
aliquots per a single random sample. In any case, the sampling decisions
should be a priori decision and should be based on the question at issue.
In addition to the number of sub samples taken for analysis, it is essential that
each be prepared in a way that achieves homogeneity and is handled in a
manner that prevents alteration from the original composition. Obviously,
failure to prepare a homogeneous sub sample at this point will affect the results
of the analysis regardless of the method used.
25
Food Analysis
11.9 SAMPLE PREPARATION FOR ANALYSIS
Every type of material that is to be prepared for analysis presents its own
practical difficulties. The requirements for suitable sample preparation are
dictated by the consistency and the chemical characteristics of the analyte and
the matrix, and by the distribution of the analyte in the sample. Even seemingly
homogeneous materials such as liquids may be subject to sedimentation or
stratification. Thus, vigilance and care are the watch words to ensure
homogenity.

11.9.1 Precautions to be followed while Preparing a Sample

for Analysis
Mixing: Single phase liquids can generally be mixed, stirred, shaken or
blended. Dry particulate materials can be reduced in the volume by coning and
quartering, by rolling and quartering, or by the use of a splitter, such as a refill.
A variety of implements and machines are available for sample disintegration,
such as mills, grinders and cutters. Care in their use is necessary to prevent loss
of dust or change in composition through partial separation of components.
Screening can be used to improve the efficiency of particle size reduction,
followed by mixing to attain homogeneity. Sampling errors can occur even in
well mixed particulate mixtures especially in trace analysis if the particles
differ appreciably in size or physical properties.

Cleanliness of equipment used in process

Every piece of equipment used in the preparation of a sample must be
examined critically to ensure their cleanliness, so that they do not contaminate
or decompose or cause any physical loss of the sample while processing.
Grinders were mentioned above as contributing to the loss of finer particles as
dust. They have been known to segregate materials with in the mix by size as
well, with the finer material, collecting beneath the blade e.g., Metal screens
can pass fine particles, but retain powder that adheres to the screen materials.
Glass containers and laboratory apparatus can adsorb certain materials and
may require surface treatment. Plastic containers can retain contaminants, such
as animal hairs, while the rest of the sample is transferred with apparent ease.
In the other words, validation of a method of analysis, includes, most certainly
validation of the method of sample preparation and storage.

Changes in physical characteristics

Loss or gain of moisture during processing can be a problem. Loss can be
minimized by keeping samples covered with plastic or aluminum foil. A cold
product can be protected from gaining moisture by allowing the sample to
come to room temperature before preparation begins. High fat samples such as
nuts may be difficult to grind without clogging up the grinder; one technique
that is used is to freeze the samples prior to grinding.
Changes in chemical characteristics
When volatile organic constituents are present in any sample, processing may
be difficult and needs special care, e.g. maintaining chilled condition to
prevent any loss of volatile constituents. Similarly, in case of photo-sensitive
chemicals (e.g. natural product pesticides), it is required to process a sample
under darkness to prevent degradation on exposure to light.
26
Portions for sampling Sampling Techniques of
Food Products
As a general guide, food samples are analyzed in the form they are commonly
consumed. Inedible portions, such as stones (e.g. for mango), nutshells, or fish
bones are removed and discarded prior to analysis, and suitable note made of
how the sample was prepared. The technique used for setting the standard
should be used to ensure comparability.

Sampling for Trace metals

Trace metals analysis can present significant problems, For example, the trace
metals can be distributed unequally between liquid and solid phases in pickles,
canned vegetables and canned fruits. Obviously, such irregular distribution of
metals can pose problems for the analyst in establishing the level of metal
residues in the product, as well as for those concerned with setting tolerances.
Thus, it becomes necessary to analyze both the solid and liquid phases.

Check Your Progress Exercise 4 "

Note: a) Use the space below for your answers.
b) Check your answers with those given at the end of the unit.
1) Write down some precautions while preparing a sample for analysis?
………………………………………………………………………………
………………………………………………………………………………
…………………………………………………………………………….…
……………………………………………………………………………….

11.10 DIFFICULTIES IN SAMPLING

As mentioned earlier, one of the most difficult problem in sampling from a lot,
and in subsequent lab subsamples, is trying to obtain a representative sample
for the analysis of aflatoxins in raw agricultural commodities. Aflatoxin
contamination exhibits a highly erratic distribution, with a reduction in
heterogeneity as the food or feed is reduced in particle size. After it was
recognized that there was a high rate of variability and within same samples
from the same lot, there was a moment towards the collection of larger and
larger samples. Sample sizes started, for peanuts with 1 kg, and the size
increased as more reliable results were required by food procedures (increasing
sample size reduces the number of good lots that are likely to be rejected and
the number of bad lots accepted).

11.10.1 Example for Effect of Sampling on Analytical Result

At the present time in the United States, the sample taken from a lot of shelled
peanuts of 144 pounds; three 48 pounds samples with portions taken at random
from the lot. Examination in the lab is by sequential analysis with first 48
pounds sample ground in a subsampling mill and test portions examined in
duplicate. If the average of the test portions is below the established tolerance
(set by US Food and Drug Administration), the lot is passed. If the average is
above the acceptance level, the lot is rejected. If the findings fall between the
two figures the second 48 pound sample is comminuted and the analysis
27
Food Analysis repeated. If a decision cannot be made to accept or reject the lot, the third 48
pounds sample is prepared, assayed, and the cumulative results considered.
The foregoing example point out dramatically the need for attention to lot
sampling, lab subsampling, and sample preparation for analysis. While this is a
rather extreme case, it illustrates that sampling problems cannot be ignored or
treated indifferently. In Canada, while the specified sample sizes are smaller,
ranging from 12 to 20 kg. depending on the commodity and the lot size, and
minimum number of sampling sites are also stipulated to address the erratic
distribution of aflatoxin contamination.

11.11 SAMPLE ACCOUNTABILITY

11.11.1 Documentation
A laboratory sample is generally the starting point for analytical work. The
sample may be delivered by mail, courier, flight, or directly by the collector. It
may arrive in any of various containers and conditions: frozen, packed in ice,
or at room temperature. The package may be sealed or unsealed, and the
sample itself may be spoiled or broken. The sample may or may not be
accompanied by appropriate documentation to advise the laboratory regarding
purpose, test parameters and the conditions of storage, etc.
Once a sample is received, all the circumstances and conditions must be
documented as they could have bearing upon the quality or the significance of
the test results. It is important for appropriate quality analysis that sample
arrives in proper condition with meaningful documents. Procedures for these
must be established, continually reviewed, and enforced, to keep poor sample
handling and delivery to a minimum level. To avoid any future legal
complications, the laboratories are advised to protect themselves with the
cautionary statement in the test report indicating that the results relate only to
the sample that was tested.

11.11.2 Chain of Custody Form

In most organizations specific sampling procedures are written and the sample
collectors are trained regarding their responsibilities. The first important
activity is the documentation to ensure product traceability. The sample should
be easily identifiable and placed under seal and packing. Shipping and delivery
instructions are followed to effect delivery to the laboratory. The
documentation consists of a chain-of-custody that accompanies the sample as it
moves through the laboratory and subsequent administrative handling. This
form is usually prepared in multiple copies for distribution to various units in
the organization, may be supplemented with affidavits, dealer’s statements,
bills or other relevant information that concerns the sample, its origin, the
transfers from one custodian to the next and the sample’s significance or
importance. Information such as sample number, product name and
identification, reason for collection, description of the sample and of the
method of collection, size of the lot from which the sample was taken, codes,
shipment information, collection date, name of the collector, means of
transportation, and whether or not sealed are supplied with the sample. If the
sample is sealed, the seal includes the sample number, date the seal was
affixed, and the collector’s signature. The seal is attached to the package in
such a way that it must be broken before the sample can be obtained.

28
11.11.3 Sample Receipt and Handling Sampling Techniques of
Food Products
The next step in the sample accountability system is receipt of the sample in
the laboratory. A dependable record of sample handling is important so that the
sample is accepted by a sample custodian who documents the action by
completing a sample accountability record. This document should contain the
sample number, the name of the product and date received, indicate who
received it, describe the method of shipment or delivery, describe the packages
received and their condition, and provide space for recording various storage
locations before and after analyses. Deliveries of the sample or portions of the
sample to the analyst, and its return, will also be recorded on this form. There
will be a signed statement concerning the final disposition of the reserve
sample. A two-part form can be used for this purpose; one copy remains with
the sample custodian and the other moves with the sample through the
laboratory and is used by a supervisor for sample management purposes. Some
laboratories use a sample receiving log book for sample control. The
information entered in the log book is essentially the same as that described for
the two-part form.

11.11.4 Monitoring of Samples

The sample accountability in a laboratory can be monitored by a simple
computer program; a unique label should be generated and affixed to the
sample container, and all the pertinent sample information should be entered
into the computer database. The information entered at log–in becomes part of
the data base, which is then built up through the manual or automatic addition
of sample handling information and analytical data. Worksheet pages or
reports can be calculated and printed, and the data base itself latter queried and
manipulated for various information and reporting purposes. Regardless of the
recording system used, the analytical information generally reported includes a
description of the sample, subsampling procedure sample preparation methods
used, deviations from methods, validation and recovery experiments (if
performed), standards used, source of reference materials, raw data,
calculations and description of the reserve sample and how it was prepared for
storage after the completion of the analysis. In addition, pertinent supporting
documents such as chromatograms, spectra, and other charts are suitably
identified with instruments identification, operating conditions, analyst name,
sample number and date. If the reserve sample is sealed, the information
placed on the seal is shown in the report. The sample is then returned to the
sample custodian to be stored for whatever future action may be necessary, or
until the sample is destroyed.

11.12 RETENTION OF SAMPLES AND RECORDS

After an analysis is complete and the results reported, the laboratory needs a
written policy for guidance on the retention of the samples and the associated
records. For samples and records that may be involved in litigation, the storage
period can extend for years. For the majority of samples, fortunately, this is not
usually the case. The objective should be to destroy samples as soon as it can
be analyzed, with certainty that they will no longer be required for further
testing or as evidence. The records may be disposed after they are no longer
legally or administratively important.

29
Food Analysis 11.12.1 Identify the Properties of Retained Samples
It is very important for the laboratory management to determine whether or not
the materials being discarded are hazardous in nature. Although samples
themselves may not be hazardous, acid digestions and organic solvent
extractions certainly can be hazardous. Sample management includes the
proper disposal of samples and laboratory preparations. Standard operating
procedures for samples for sample disposal are essential.

11.12.2 Retention Period

Storage periods, obviously, must be determined by each facility depending on
its obligations, but clear policy must be in place to prevent both the destruction
of important items, and the accumulation of what is essentially junk. From a
quality assurance point of view, the improper destruction of active samples or
records is low quality performance in violation of policy, and the Quality
Assurance (QA) program must provide a means to detect such actions in an
effort to prevent their recurrence.

11.13 CASE STUDY

In a 500 T consignment of imported frozen animal carcasses, 300 T labeled as
produced by A and 200 T labeled as produced by B is to be checked for
residues.
Assumed facts:
i) The carcasses are from an exporter whose products have recently been
associated with excessive residues of Permethrin (fat soluble) and
Diflubezuron (non-fat soluble).
ii) Carcasses in lot A have trimmable fat, where as those in lot B do not.
iii) The sampling plan is to provide a 95% probability of detection if 10% of
the carcasses contain excessive residues.
iv) There is no legal requirement to prepare replicate lab samples.
v) Sampling records are in hard copy form.
vi) Rendering of fat tissue for extraction of lipid acceptable under national
law.
Consequent actions and discussions:
i) The consignment is sampled as two separate, suspect lots, A and B
ii) Table 11.3 shows that 29 lab samples should be taken and therefore, as
far as practicable, 29 carcasses are selected at random from each lot.
iii) From each selected carcass in lot A, a minimum of 0.5 kg of adhering
fat tissue is taken as a (primary) lab sample and a minimum of 0.5 kg of
meat (meat does not include bone) is taken as a separate (primary) lab
sample.
iv) The carcasses in lot B have no trimmable fat and 29 samples of 2 kg
meat are taken.
v) As each lab sample is taken, it is placed in a new polythene bag,
securely labeled and sealed, and the sample record completed. The
samples are sent to the lab, ensuring that they do not thaw.

30
 Copies of the sample records are given to the owner/custodian of the Sampling Techniques of
consignment. Copies are sent with the samples and also retained by the Food Products
sampling officer.
vi) Fat tissue lab samples from lot a are rendered, the lipid collected and
aliquots (analytical portions) analyzed for Permethrin residues. The
results are expressed on a whole fat tissue basis.
vii) Bones, if any, are removed from the meat lab samples, which are
minced before the determination of Diflubenzuron residues in
analytical portions. The results are expressed on the basis of whole
meat without bones.
viii)If meat samples from both lots contain Diflubenzuron ≤ 0.05 mg/kg
and all samples from lot A contain < 1 mg/ kg Permethrin, lot B is
acceptable and lot a is acceptable with respect to Diflubenzuron
residues.
ix) If 3 of the 29 fat samples of lot A contain Permethrin > 1 mg/kg,
replicate analytical portions of fat from these 3 lab samples are
analyzed. Taking into account the analytical uncertainty, if the results
conform that the MRL is exceeded, if the 3 carcasses do not comply
with the MRL, where as the other 26 do comply with the MRL.
x) If the entire lot is not to be rejected on this basis, lab samples of fat
tissue from the remaining carcasses in lot A may be taken for analysis,
in order to separate the acceptable carcasses for those that are
unacceptable.

11.14 LET US SUM UP

Actions for the management and control of sampling, sample preparation, and
sample analysis are summarized below:
1) Work with appropriate persons to develop sampling plans for the various
types of products delivered to the laboratory for analysis.
2) Establish sub sampling procedures for various products, giving
consideration to the use of composites or individual unit examinations,
based on the variability to be expected among sample units and the
resources available for their analysis.
3) Prepare guidelines for sample preparation for analysis that will minimize
composition change.
4) Choose the appropriate sampling selection method to achieve the intended
purpose of taking samples.
5) Describe subsampling within the lab in written procedures which analysts
have the responsibility to follow.
6) Manipulation and preparation must be done with care to avoid losses of
material.
7) Develop a system to ensure sample accountability.
8) Provide policy for the management of samples when they are no longer
needed.

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Food Analysis 9) Maintain written procedures for sample disposal taking into consideration
hazardous waste regulations.

11.15 KEY WORDS

The definitions of sampling terms used in this document are mostly those
specified in ISO 7002. Some of the more commonly used terms in acceptance
sampling are described in this section.
Lot : A definite quantity of some commodity
manufactured or produced under conditions, which
are presumed uniform for the purpose of this
document.
Consignment : A consignment is a quantity of some commodity
delivered at one time. It may consist in either a
portion of a lot, either a set of several lots.
Sample : Set composed of one or several items (or a portion of
(Representative matter) selected by different means in a population
sample) (or in an important quantity of matter). It is intended
to provide information on a given characteristic of
the studied population (or matter), and to form a
basis for a decision concerning the population or the
matter or the process, which has produced it.
A representative sample is a sample in which the
characteristics of the lot from which it is drawn are
maintained. It is in particular the case of a simple
random sample where each of the items or
increments of the lot has been given the same
probability of entering the sample.
Sampling : Procedure used to draw or constitute a sample.
Empirical or punctual sampling procedures are
sampling procedures, which are not statistical-based
procedures that are used to make a decision on the
inspected lot.
Total Estimation : In the estimation of a parameter, the total estimation
Error error is the difference between the calculated value
and the true value of the parameter. The total
estimation error is due to:
i) Sampling error ii) Measurement error
iii) Rounding-of-values vi) Bias of the estimator
or sub-division
in to the classes
Sampling Error : Part of the total estimation error due to one or
several of the following parameters:
• The heterogeneity of the inspected characteristics.
• The random nature of a sampling.
• The known and acceptable characteristics of the
sampling plans.

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 Sampling Techniques of
Acceptable Quality : The inspection of a lot using either an attributes or Food Products
Level (AQL) variables sampling plan will allow a decision to be
made on the quality of the lot.
AQL for a given sampling plan is the rate of the non-
conforming items at which a lot will be rejected with
a low probability, usually 5%.
Limiting Quality : For a given sampling plan is the rate of non-
(LQ) conforming items at which a lot will be accepted
with a low probability, usually 10%.
Sampling Plan : A pre-determined procedure for the selection,
withdrawal, preservation, transportation and
preparation of the portions to be removed from a lot
as samples.

11.16 ANSWERS TO CHECK YOUR PROGRESS "

EXERCISES
Check Your Progress Exercise 1
Your answer should include following points:
1) The quality of a small sample analyzed is attributed to the lot, which the
sample represents. If the sample does not represent the population
adequately and efficiently, then the results obtained may not truly represent
the quality of the lot.
2) Homogenous population would be uniform and identical at all locations.
These populations/samples in which the composition would vary at
different locations is heterogenous population.
Check Your Progress Exercise 2
Your answer should include following points:
1) It is very important to arrive at a well designed sampling plan because it is
a guide to the people who are going to perform sampling. It also serves as a
reminder of the important elements in the over all analytical program.
2) a) Sampling plan is a guide for the whole analytical program.
b) It is a means for operating on a planned basis which reduces variation.
c) It serves as a reference document for similar activities in the future.
d) A document for comparison of performances against objectives.
e) It also serves as a source for imparting training.
Check Your Progress Exercise 3
Your answer should include following points:
1) i) Probability sampling,
ii) It is a means for operating on a planned basis which reduces variation,
iii) Non-Probability sampling,

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Food Analysis iv) Bulk sampling,
v) Acceptance sampling,
vi) Sampling by attributes, and
vii) Sampling by variables.
2) Probability sampling is used when a representative sample is desired, and
uses principles of statistical sampling and probability, a random selection
approach that tends to give each unit an equal chance of being selected.
3) Sampling by attributes:
Advantages: 1. No condition on the mathematical law of distribution of the
variable inspected. 2. Greater simplicity of the processing the results on the
sample.
Disadvantages: 1. Less effective than variables plans for a same sample
size of n increments (Least Quality, LQ is higher). 2. More costly than
variables plans because the collected sample requires more increments than
those required, for the same efficacy, by a variables plan.
Sampling by variables:
Advantages: 1. More effective than attributes plans for the same sample
size of n increments (LQ is lower) for the same AQL, they are less
expensive than attributes plans because the sample collected requires fewer
increments than those required for a same efficacy, by attributes plans.
Disadvantages: They cannot be used in all cases because to validate the
calculation formulas of the inspected variable must necessarily or
approximately follow a normal law.
4) Set the values of m, M, n and c → Collect the sample with n items →
Inspect each item in the sample → Accept the lot if: number of marginally
defective items (i.e. a concentration of micro-organisms between m and M)
≤ c. Immediately reject the lot if the concentration of the micro-organisms
in any item > M and / or the number of marginally defective items > c.
Where, m: accptable concentration; M: unacceptable concentration;
c: maximum allowable number of marginally acceptable sample units; and
n is the number of sample units selected randomly from the lot.
5) a) The lots shall be thoroughly inspected before sampling to design a good
sampling plan.
b) Suitable sampling devices shall be identified and used while sampling.
c) Compatible containers shall be identified and used. The material of the
container shall not cause any undue contamination to the quality of
sample collected. For example, Non-sterile containers shall not be used
while the sample has to undergo microbiological tests.
d) Suitable packing and delivery method.
e) Provision of appropriate environmental conditions. For example, When
there is a need to determine Volatile Organic Constituents in a sample
of water, it has to preserved/transported at a temperature 4 to 8oC.
6) Root and bulb vegetable- 5 kg, cereal grains- 2 kg, poultry eggs- 12 eggs,
liquid milk- 0.5 L, liquid products- 0.5 L

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Check Your Progress Exercise 4 Sampling Techniques of
Food Products
Your answer should include following points:
1) a) Use a suitable method for homogenization. For example, Liquids can
be homogenized by stirring, shaking or by blending and take an aliquot.
Solids can be homogenized by grinding, pulverizing and volume
reduced by coning and quartering.
b) Use clean and suitable sampling devices and containers. For example,
A scoop used for sampling a food shall be sterile.
c) A glass container is not compatible for collecting water sample
intended for the determination of metals, since metals like sodium are
absorbed by glass.
d) Moisture content of sample changes with surrounding temperature.
Suitable precautions shall be taken to retain the originality.
e) Maintain suitable environmental conditions to minimize expected
chemical changes if any. For example, A food sample for
microbiological enumeration shall be collected in a sterile container
and be stored/transported in chilled condition.
f) If the sample is presented in both liquid and solid phases, homogenize
both phases before a test portion is taken.

11.17 SOME USEFUL BOOKS

Nielsen, S. Suzanne (2003). Food Analysis Laboratory Manual, 3rd Edition,
CHIPS Publishers, U.K.
International Organization for Standardization (ISO): www.iso.org
Codex Alimentarius (CODEX), www.codexalimentarius.net
Agriculture and Processed Food Products Export Development Authority
(APEDA), Ministry of Commerce and Industry: www.apeda.com
Bureau of Indian Standards (BIS), Ministry of Consumer Affairs, Food and
Public Distribution: www.bis.org.in / www.fcamin.nic.in
Export Inspection Council of India (EIC), Ministry of Commerce and Industry:
www.eicindia.org
Prevention of Food Adulteration Act (1954), 24th Edition, 2003, Ministry of
Health and Family welfare: www.mohfw.nic.in

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