ICUMSA News n°25 – 1995

Message from the President

It is now more than one year since our Havana meeting. We have the 21st Session Proceedings, so the work of the 22nd Session can now begin in earnest. I would like to draw attention to the need to have more of our methods collaboratively tested. We enjoy widespread recognition as the authority on sugar analysis, but we run the risk of losing that if we do not have our methods accepted by accreditation agencies. Our highest priority should be directed toward the methods used in commerce. Our next priority should be to ensure that all new and emerging methods be properly tested to satisfy both ourselves and users that these methods are robust.

We anticipate issuing our first supplement to the Methods Book in 1997 and we should attempt to have a significant amount of our collaborative testing work completed so that it can be included in that revision. I look forward to an outstanding effort on collaborative testing in this the Session leading up to our Centenary.

Laboratory accreditation and some notes on General Subject 4: Molasses

Clive J. Shelton, Referee

The UK organisation for laboratory accreditation, NAMAS (the National Measurement Accreditation Service), formerly administered by the Department of Industry, has been made an executive agency and is now run along company lines. NAMAS is the UK’s certification body for the purposes of the EN45000 series of standards and a key member of WELAC, the Western European Accreditation Conference. The “privatisation“ of the service has been followed this year by the merger with the National Accreditation of Certification Bodies organisation (NACCB). This latter body assess certification bodies who certify quality management systems to the BS EN ISO 9000 series of standard. They also assess bodies who offer product certification and personal certification. The merged body will be launched in 1995 and will be operated as a company limited by guarantee.

The merger is in line with European practice. Although the UK has many years of experience in accreditation, it is a much newer concept in other European countries. The European Commission has encouraged the development of nationally recognised accreditation bodies throughout Europe and most member states now have similar bodies to NAMAS and NACCB.

The use of quality systems in laboratories is not new. The requirements of the EN45000 series go further than the internationally recognised ISO 9000 system, however. NAMAS requires not only that laboratories have a written quality system to which they adhere. The system must include key policies including those for training, qualification, provenance of methodology, calibration, reporting etc. and the system as a whole is assessed by experts in the field for which the laboratory is applying for accreditation. In this way the laboratory can be sure that its procedures are assessed as up-to-date, relevant and accurate.

NAMAS often insist on laboratories performing satisfactorily in performance assessment schemes run throughout Europe. This is in addition to internal quality control monitoring, which all laboratories must carry out. In the UK, the Ministry of Agriculture run the so-called FAPAS scheme and members will be aware of this initiative through the work of Roger Wood (Member of the British National Committee of ICUMSA). This has become doubly important in the European Union due to Directives from Brussels which prescribe that official food law enforcement laboratories perform satisfactorily in such schemes. Laboratories are submitted samples and instructed to perform various analyses according to their in-house procedures. Results are returned and the performance of laboratories assessed against other participants in terms of the mean of all laboratories. In some fields, particularly instrumental methods, “expert“ laboratories are identified and used as the benchmark for comparison of other laboratories.

On more specific matters, I have begun to prepare the documentation for an international collaborative excursus on General Subject 4 methods of analysis. I shall be writing to various laboratories in due course but would ask that those interested in participation should contact me directly. I shall be including all of the copper reduction methods for Cane and Beet molasses, as well as polarimetry and moisture determinations. I would like to include comparisons between vacuum sand drying and Karl Fischer moisture determination, as agreed in Cuba, and request that laboratories indicate whether they have the necessary equipment for this.

Progress report on Subject 5: Dry Substance

G. Vaccari, Referee

Bearing in mind the Recommendations adopted in Havana as far as Subject 5 is concerned (ICUMSA News No. 22, September 1994), the Referee is trying to get in touch with the Associate Referees and other laboratories which might be involved with the objective of organising some collaborative tests.

Because we should be using more modern methods of analysis and in particular methods which are more rapid than the oven drying method for both sugar and other sugar products, the utilisation of modern Karl Fischer titration (without using pyridine), infrared radiation methods and NIR spectrophotometry have been suggested.

Regarding the KF method, Mr. Faviell (Canada) has written up the latest KF method in ICUMSA format as methods for the analysis of Raw Sugar, Specialty Sugars, Molasses, Cane Syrup & Molasses in Cane Sugar Processing and for the determination of Moisture in White Sugar. Such methods should be included in the ICUMSA Methods Book, but to become Official they have to be validated via a Ring Test. In this work on molasses we will collaborate with Mr. Shelton (UK) and Mr. Faviell is kindly at our disposal for sending to the laboratories involved the relevant samples of the various products, in particular the cane products.

Regarding infrared radiation methods to determine sugar moisture content, Mr. Caulkins (USA), who is particularly keen on this type of method (e.g. using the Omnimark instrument), is available to give us all the details of the method and to set up a ring test on the application of such a methodology.

Mr. Parkin (UK), the Referee for General Subject 2: White Sugar, suggests that if it is possible to carry out both the tests of the KF and IR methods for white sugar, the same samples should be utilised for both methods. Mr. Parkin’s laboratory would also be the reference point prepared to utilise the Official ICUMSA Method GS 2/1/3-15 for the analysis of the samples to be circulated.

Concerning NIR spectroscopy, the Referee is asking the opinions of the Associate Referees about the possibility of organising a ring test, taking into account that each instrument needs a proper calibration. The Referee thinks that before organising a ring test the participants should receive samples of the various products having known dry substance contents so that everyone could prepare the relevant calibration curves. Only after the evaluation of such curves could the ring test be organized.

As soon as the Referee receives the agreement of a sufficient number of participants willing to take part in the ring tests can these tests be organized according to the suggestions made by the Referee for Subject 3, Mary Ann Godshall, and reported in ICUMSA News No. 23, January 1995.

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