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determining carbonate in washing powder | laboratory talk

In recent years the cost of ion chromatography instruments has fallen drastically and they now represent a cost effective and rapid alternative to titrimetric methods that are currently widely used for carbonate analysis.

They have to deliver high standards of cleaning, be safe towards people, fabrics and the environment. Carbonate present as sodium carbonate is a key component in washing powders, and the manufacturers of such products require a simple yet reliable way of quantifying its presence to ensure that quality control tolerances are maintained.

Non ionic detergents generally consist of condensation products of alcohols or phenols with ethylene oxide. The builder in washing powders enhances the effect of the surfactant by deactivating calcium and magnesium ions which would otherwise use up the surfactant molecules.

Builders are water softeners and work by complexation (eg, sodium tripolyphosphate or nitriloacetic acid), precipitation (eg, sodium carbonate) or ion exchange (eg, zeolites); most of them produce alkaline solutions which aids the cleaning as most detergents work effectively around pH10-11.

Fillers are materials added to washing powders to alter their physical properties - like making the powder more free flowing (as is the case of sodium sulphate), or to lower the freezing point (as for alcohols and liquid detergents).

Bleaches (often sodium perborate) are added to bleach coloured stains that are not easily removed by washing, but these work effectively only at temperatures above 60C - so activator compounds such as tetra acetyl ethylenediamine are added, which lower the temperature at which the bleach operates.

Their function is to offset the yellowing of white cottons and linens by absorbing ultraviolet light and re-emitting it as visible light in the blue region, increasing the total amount of light reflected by the surface to give a 'whiter white'.

Enzymes are added to biological detergents as catalysts to help break down biological stains, such as blood and grass marks, that may be present on the fabrics, thus making it easier for the other ingredients present in the washing powder to lift the dirt away from the clothing. Fabric softeners impart softness to the human touch by controlling the amount of static electricity that is present in the washed article; typically these are quaternary ammonium compounds.

A corrosion inhibitor like sodium silicate is added to reduce corrosion of the appliance surfaces, and is incorporated into washing powder to protect the metal parts and finishes inside the washing machine.

Colourants and fragrances are added to improve the appearance of the washing powder, and give the washed garments a distinctive aroma in character with the product, as well as masking any unpleasant odours from the wash water.

Industrially, sodium carbonate is referred to as soda ash and is produced in two grades; light ash (a fine powder) and heavy ash which has a bigger particle size and is denser, making it more efficient to transport.

To a solution of brine (sodium chloride in water), ammonia is added followed by carbon dioxide - resulting in the precipitation of sodium hydrogen carbonate that decomposes to sodium carbonate when elevated to a temperature of 175C.

The role of sodium carbonate in washing powder is crucial; it may be used as a water softener and it is also used to raise the pH of the detergent as other ingredients that are present in the washing powder (particularly zeolites) tend to work better at elevated pHs.

Hard water tends to fur pipes as a result of the carbonate formed during heating, and more washing powder is required for washing as the hard water forms a scum with calcium or magnesium compounds formed with the detergent.

Chromatography is a method for separating mixtures of substances using two phases, one of which is stationary and the other mobile moving in a particular direction. Chromatography techniques are divided up according to the physical states of the two participating phases.

A general definition of ion chromatography can be applied as follows: "ion chromatography includes all rapid liquid chromatography separations of ions in columns coupled online with detection and quantification in a flow-through detector".

In ion chromatography without chemical suppression (direct ion chromatography) very high demands are placed on the conductivity detector since the background conductivity (which must be compensated for) is relatively large in comparison with the measured signal.

Of prime importance for electronic suppression is the constancy of the background, and as conductivity is extremely temperature-dependant, a good temperature constancy of the eluent flowing in the detector measuring cell is required (<0.01C). The sensitivity of conductivity measurements depends on the difference between the equivalent ionic conductivities of the sample and eluent ion.

Thus, should an anion with a higher equivalent ionic conductivity appear in the detector cell, the conductivity will increase and a positive peak will be observed and recorded by the data acquisition software.

25mg of the dried analytical sample was weighed accurately into a 100ml volumetric flask before being diluted up to the mark with deionised water. The sample was sonicated for a period of ten minutes in an ultrasonic bath, to aid homogeneity of the sample as well as removing carbon dioxide.

The diluted sample was injected into the Metrohm 761 Compact IC through a RP sample preparation cartridge, and the response for the peaks recorded using an eluent of P-hydroxybenzoic acid/acetonitrile with the Metrohm Super-Sep analytical column.

The 761 Compact IC comprises a low-pulsation dual-piston pump, pulsation dampener, electromagnetic injection valve, two channel peristaltic pump (optional, not required for carbonate analysis), suppressor module (optional, not required for carbonate analysis), conductivity detector, eluent organiser as well as a data recording and processing module.

The detector is the heart of every ion chromatograph. Metrohm says its detector's temperature varies by less than 0.01C and can be optimally adapted to the ambient conditions. This outstanding temperature stability reduces interference and allows exact conductivity measurements.

When a large sample throughput is required, it is recommended to automate the ion chromatograph with one of the following Metrohm auto samplers: the 766 IC sample processor, the 788 IC filtration sample processor, or the 813 compact autosampler.

Ion chromatography as an analytical technique has seen an enormous surge in popularity, due partly to the simplicity of many of the methods as well as other factors such as market forces driving down the expenditure costs of the equipment and an improved instrument power.

The running costs of ion chromatography with Metrohm instruments are surprisingly low, says the company, requiring only the acquisition of chemicals required for the eluent as well as a clean, reliable source of deionised water for preparation of the standards and samples. With Metrohm ion chromatography systems it is possible to work non-suppressed, giving the analyst the option to run applications like carbonate using IC as opposed to current titrimetric methods.

If, after the analysis has been completed, it is necessary to perform a suppressed anion application, then all one has to do is attach the suppressor module between the separation column and detector to change the chemistry of the Metrohm IC system.

Its robustness and reliability are assured, demonstrating precisely the reason why it is rapidly becoming the method of choice for many analysts in a plethora of different industries and is eminently suited to the analysis of carbonate in washing powder.