Starch granules can often be distinguished by their shape, size distribution, hilum and lamellae; dextrin and inulin are distinguished chiefly by their molecular constitution, solubility and chemical reactions. An isolated particle of uncertain origin cannot always be identified uniquely by one feature.
In a water-mounted preparation of unheated starch, potato granules are usually relatively large, oval or pear-shaped, often with an eccentric hilum near the narrower end and conspicuous curved growth markings. Wheat gives a characteristic mixture of larger flattened lenticular granules and small rounded granules; the hilum and rings are less conspicuous. Rice starch consists of very small angular or polyhedral granules, often still associated into compound groups. These are distributions rather than a guarantee that every potato granule is larger than every wheat granule.[ref]
Starches in The International Pharmacopoeia. Microscopic identification: potato, wheat and rice granule shape, hilum and striations
Maize commonly gives polygonal or rounded granules with a central point or fissured hilum; oats characteristically include aggregates of small angular granules. Arrowroot commonly has oval or elongated granules, sometimes with a transverse fissure towards one end. Preparation, variety and processing change the apparent population. Rotation between crossed polarizers shows the organized granule structure through a characteristic extinction cross in many intact granules. Swelling and loss of birefringence on heating with sufficient water help demonstrate starch gelatinization, although the precise temperature depends on the starch source.
Cold water normally leaves native starch granules as a suspension rather than a clear molecular solution. On heating, granules swell and a paste develops. With iodine in iodide solution, ordinary starch rich in sufficiently long amylose helices produces an intense blue or blue-black complex. Its intensity depends on chain structure and conditions; the response can weaken on heating and return on cooling if the chains remain suitable. Continued acid or enzymatic hydrolysis shortens chains and eventually destroys this characteristic blue response.
Dextrin denotes a range of shorter or modified glucose polymers derived from starch, rather than one pure substance. Many preparations dissolve or disperse in water more readily and no longer show intact native granules. Their iodine reactions vary with chain length: some give violet or reddish-brown colours, while extensively shortened material gives no characteristic colour. It is therefore too absolute to say that every dextrin is chemically identical or that no dextrin can react with iodine. The modern international specifications themselves distinguish starch modifications and their variable iodine colours.[ref]
Dextrins in MeSH. Definition: mixtures of glucose polymers produced by starch or glycogen hydrolysis
[ref]Modified Starches: Specifications by the Joint FAO and WHO Expert Committee on Food Additives. Identification; iodine colours and hydrolysis test in the specifications summary
Inulin is principally a fructose-based fructan, with a different linkage pattern from glucose-based starch. It occurs, for example, in chicory and related storage organs. It does not give starch's blue iodine complex. It dissolves more readily in hot water, and may separate as deposits on cooling or precipitation, but such deposits are not the characteristic native starch granules. Hydrolysis yields mainly fructose, whereas complete starch or dextrin hydrolysis yields glucose. A copper-reduction test after hydrolysis detects reducing products in both cases and is therefore insufficient by itself to distinguish them. Their different hydrolysis products, interpreted with iodine reaction and microscopy, give a more specific comparison.[ref]
A sound comparison uses separately labelled reference preparations, equal iodine conditions and separate unheated and heated mounts. Inspecting an unknown mixture only after boiling destroys much of the morphological evidence. The combined observations distinguish source-related morphology from the effects of processing.
In a period account of bread adulteration, give first place to alum, then distinguish undeclared flour or starch substitutions, water-retaining additions, and alleged mineral or metallic adulterants. Their actual occurrence must be demonstrated; a long list in a textbook is not proof that every loaf contains them.
Alum was added to alter the appearance and baking behaviour of inferior flour and to help produce an apparently acceptable white loaf. It is the especially well-supported English example. Arthur Hill Hassall's 1855 investigations reported alum in two series of bread samples, while finding neither potato nor other foreign flour in those series. The same work found none of the suspected mineral fillers in its examined series of forty-four flour samples. These are observations about the samples examined, not a warrant to declare all English bread adulterated.[ref]
Food and Its Adulterations by Arthur Hill Hassall. 1855, Introduction, conclusions on bread; “Bread, and its Adulterations”, p.143, analyses of forty-four flour samples
The organic substitutions to consider include potato or potato starch, and cheaper flours from rice, maize, rye or beans. Their economic significance is the substitution of a different material for flour sold as wheat, rather than the proposition that every such food is intrinsically poisonous. A declared mixed-grain loaf is a different case from concealed substitution. Defective or damaged flour can also be disguised through additions that improve apparent texture or colour. Moisture matters because a loaf retaining excessive water can deliver less food material for the same purchased mass.
Historical reports also discussed chalk, gypsum or plaster of Paris, clay, magnesia and other mineral fillers, together with copper(II) sulfate, or “blue vitriol”, as a baking addition. These should be presented as reported or suspected adulterants of bread or its flour, with prevalence qualified. An 1851 contemporary review gives the broad period list; the later direct analyses show why allegations require testing.[ref]
The Commercial Hand-Book of Chemical Analysis in The British and Foreign Medico-Chirurgical Review (1851). Review passage headed “Bread”: starch substitutions, alum, chalk, blue vitriol, magnesia, clay and plaster of Paris
The comparison can be made experimentally. Examine flour particles with a microscope for foreign starch granules and plant tissues, comparing reference materials; baking disrupts many structures, so unbaked flour is often more informative than a cooked crumb. Determine moisture by drying a weighed portion, and examine the ash for unusual inorganic residue. Neither excess ash alone nor a metal detected in trace quantity identifies the material added or its intention. Sampling, blanks and the natural composition of flour must be considered.
In particular, testing for alum requires distinguishing introduced material from naturally present mineral constituents and from contamination of the reagents. A pre-examination 1865 review explicitly criticized analytical errors in separating aluminium compounds from bread ash and disputed the claim that alum was invariably present. Thus the answer should name the principal adulterants while keeping the strength of the evidence visible. It should not repeat historical claims of harm as modern toxicological conclusions without an appropriate exposure assessment.[ref]
Sanitary Science and Legislation in The British and Foreign Medico-Chirurgical Review (1865). pp.37–38, discussion of alum in bread, phosphate interference, reagent contamination and disagreement between analytical surveys