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IUE Commission

Dr S Rajamani - Chairman
Central Leather Research Institute, Adyar
Chennai 600 020
India
Tel/Fax: +91 44 491 6351
Email: rajamani@gaismd01.vsnl.net.in

Minutes of the Joint IUC/IUE/IUF/IUP Meeting
30 May 2003
Presidente Intercontinental Hotel, Cancun, Mexico

The meeting was postponed for the original scheduled time of 1200 hrs to allow the completion of the morning presentations and was eventually called to order by the Chairman, Dr C T Page, at 1300 hrs.

Attendees:

Patricia Casey Argentina
Catherine Money Australia
Alexandre Finkler Brazil
Mariliz Gutterres Brazil
Regina Canovas Teixeira Brazil
Anne-Laure Hans France
Thierry Ponchet France
Heinz-Peter German Germany
S Rasamani India
Lluisa Cabeza Spain
Agustin Marsal Spain
Campbell Page Switzerland
John Williams UK
Stella Cristobel Uruguay
Mainul Haque USA
Elton Hurlow USA
Luis Zugno USA

As an introduction it was explained that this meting was called specially to inform Members of the activities of the IU Commissions, in particularly for those Members who are normally unable to attend Commission meetings.

1. Report of the IUC Commission - Dr A J Long
Dr Long was unable to attend but she had prepared a report which was presented on her behalf by Dr C T Page.

The last meeting of the IUC commission was held at BLC, UK on Wednesday 11th September 2002. Below is a brief summary of the points discussed along with a summary of any progress since. The report also includes progress within the European CEN/TC 289/WG2/TG1 (Chemical Test Methods).

Draft IUC 18 - Determination of chromium VI content
This method is based on a method recently accepted as a Technical Specification (CEN/TS 14495) The aim being that the method would stand as a voluntary standard for up to 3 years. During the enquiry stage many comments were received concerning the method, many of a minor editorial nature, which were accepted. On a more technical note it was decided to remove all references to the need for conditioning the samples prior to analysis. All leathers should be analysed for total volatile content (according to IUC5) and results quoted on leather weight at 0% moisture.

The detection limit of the method was raised, and it was agreed that an extra paragraph was required to indicate that leather extracts are a complex matrix and that results below 10ppm are highly variable. These would therefore be considered unreliable.

This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting.

It was suggested that there was no need for the solid phase extraction of the blank solution. This comment was accepted and an amendment will be required:

· Section 7.4 Change last sentence to read "The blank solution is treated in the same way as the analytical solution, but excluding the solid phase extraction step"

Draft IUC 19 - Determination of formaldehyde content of leather
This method has also recently been accepted as a CEN Technical Standard (CEN ISO TS 17226).

As with the Cr VI method some amendments have been discussed and changes agreed. An extra paragraph has been included in the scope to highlight that the Part A and Part B will not necessarily give identical results.

The HPLC conditions were highlighted as being recommendations only, but that validation should be carried out to ensure recovery rates detected were adequate.

Reference to conditioning of the leather was removed from the text as it was agreed that the benefits from increased accuracy of the results would be masked by the variability of the test method.

This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting. Some comments have been received and as a result the following amendments are required of the method.

· Section 5.5.4 1st three paragraphs should read as follows:
'2,5 ml (see Note 1) of the filtrate obtained in 5.6.2 is pipetted into two 10ml volumetric flasks. Add to one volumetric flask an exactly determined volume of the formaldehyde standard solution for calibration (5.6.6), which will lead to approximately the same concentration as was found in the sample (see Note 2). Both volumetric flasks are filled with water to the mark.

The contents of the volumetric flasks are then transferred to separate 25 ml Erlenmeyer flasks, 5ml of reagent solution (5.3.2) is added to each and stirred for 30 min ± 1 min at 40°C ± 1°C.

After having cooled down (protect from light), a measurement of the absorbance (5.4.4) is taken at 412 nm against a blank made of 5ml of detergent solution (5.3.1) + 5 ml reagent solution (5.3.2). The absorbance of the spiked sample will be registered as EA. The absorbance of the un-spiked sample is recorded as EP.'

· Section 5.5.4 Note 2. Should read '….then spike with 0.5ml of formaldehyde
standard solution (5.6.6)'
· Section 5.5.4 'Czu' in equation should read 'Ezu'

· Section 5.5.4 Final sentence should read 'If the recovery rate (RR) is not between
80% - 120% the analysis should be repeated.'
· Section 5.5.4 Renumber as 5.6.8
· Section 5.6.2 '2g ± 0.1mg leather' should read '2g ± 0.1g leather'
· Section 5.6.6 2nd paragraph, 3rd line '74mg/kg' should read '75mg/kg'

Draft IUC 20 - Determination of certain azo colourants in dyed leathers
The method for azo-dyes determination has recently been accepted as a technical standard through CEN (CEN/ISO TS 17234). The comments circulated to CEN were discussed and it was agreed to remove the need for conditioning the leather.

This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting. The following amendments are required for the method:

Section 4 Move last sentence to a new paragraph.
Section 5.2 Add '…capable of maintaining 70°C ± 2°C'
Section 5.10 Delete hyphen
Section 5.11 Change DC to TLC
Section 6.7 Change 6.6 to (6.6)
Section 6.7 Delete brackets after colon
Section 6.8 change 6.6 to (6.6)
Section 6.8 Delete brackets after colon
Section 6.10 Add at end '..freshly prepared from stock solutions (6.7) or (6.8) depending on the analytical method'
Section 7. Change 'together with' to 'in'
Section 8.1 Change last sentence to 'The residual hexane in the ground leather
sample is evaporated…'
Section 9 Change to 'The standard solution (6.10) with 30 mg/ml is used for calibration.'
Section 11 Change end of 1st sentence to read '…reference to the 30 mg/ml
standard solution of amines (6.10)'.

Draft IUC 21 - Determination of certain azo colourants in dyestuff mixtures

This procedure has been prepared by the IUC Commission to provide an analytical method for those wishing to check azo dyes for forbidden amines.

This method has been published in JSLTC for comment prior to voting at the delegates meeting. The following amendments are required for the method:

Section 4 Move last sentence to a new paragraph.
Section 5.2 Add '…capable of maintaining 70° C ± 2° C'
Section 5.10 Delete hyphen
Section 5.11 Change DC to TLC
Section 6.7 Change 6.6 to (6.6)
Section 6.7 Delete brackets after colon
Section 6.8 change 6.6 to (6.6)
Section 6.8 Delete brackets after colon
Section 6.10 Change to read after bold print '300mg amine / ml methanol, freshly prepared from stock solutions (6.7) or (6.8) depending on the analytical method'
Section 9 Change to 'The standard solution (6.10) with 300 mg/ml is used for calibration.'
Section 11 Change end of 1st sentence to read '…reference to the 300mg/ml standard solution of amines (6.10)'
Section 13 Change 'p-Cresidine' to '4- Cresidine'

Draft IUC 25 - Determination of PCP in leather
The method for PCP has recently been accepted as a technical standard through CEN (CEN ISO 14494). The comments circulated to CEN were discussed and it was agreed to remove the need for conditioning the leather (as with IUC 19).

The type of detector specified by the method is currently ECD. This has historically been the most sensitive detection system for this type of analysis. Due to advances in modern analytical equipment it was suggested that GC - MS be included also. It was agreed during the meeting to change the wording to 'any suitable detection system'; however at a subsequent meeting of CEN TC289 it was suggested that this may be too vague, with no reference to a validation system. For this reason the final draft specifies ECD and GC-MS.

The title of the method has also been amended to be consistent with the other methods. This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting.

Draft IUC 5 - Determination of volatile matter
It was suggested that this method should include a reference to IUP 3 Conditioning, however it was agreed that this would not be appropriate. Conditioning would alter the volatile content of a sample. An analytical balance was included into the apparatus required. This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting.

Draft IUC 6 - Determination of water soluble matter, water soluble inorganic matter, and water soluble organic matter.
This method is also currently progressing through the CEN system. The method is approved for public enquiry. The comments proposed from the CEN committee were accepted. This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting

Draft IUC 8 - Determination of chromic oxide content.
The results of the CEN public enquiry from this method have recently been sent to the IUC commission. These were discussed at the last IUC meeting, however it was decided that the method in its current state is too complex. Dr Long agreed to redraft the method to separate the sample preparation from the analytical technique. Also guidance as to the applicability of the methods for certain levels of chromium content would be included. It is intended that this will be discussed further at the next full meeting of the IUC commission.

Draft IUC 22 - Determination of the Aluminium oxide content of aluminium tanning agents
This method was published in JSLTC some time ago and comments were received via the SLTC technical sub committee. These were discussed and agreed. This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting

Draft IUC 23 - Determination of the pH of aqueous solutions of aluminium tanning agents
This method was not considered to be useful to the industry and therefore it was agreed by the committee to abandon the method. No further work will be done with this test method.

Draft IUC 24 - Determination of the basicity of aluminium tanning agents.
This method was published in JSLTC some time ago and comments were received via the SLTC technical sub committee. These were discussed and agreed. This method has subsequently been published in JSLTC for comment prior to voting at the delegates meeting

Summary
From the above it is clear that considerable work has been carried out related to the test methods in progress. It is hoped that these may be accepted at the delegates meeting at this conference. As a result the only outstanding method will be IUC 8, Determination of Chromic Oxide Content.

For this reason it now prudent to consider the future work of the IUC commission.

Proposed new methods for investigation.
The requirement for methods to determine organo-tin compounds, pesticides and chlorinated phenols has been discussed.

In each of the areas it was considered important for an industry standard test method to be agreed. Comments from those attending this meeting would be appreciated with regards to these or other methods considered of value to the industry. Any information related to test methods in this area would be appreciated as discussion points for the future.

2. Report of the IUE Commission - Dr S Rajamani
The IUE is an important commission of IULTCS. It is actively functioning with membership from nearly 25 countries. The representations are from:
1.Argentina, 2.Austria, 3.Australia, 4.Brazil, 5.China, 6.Colombia, 7.Czech Republic, 8.Denmark, 9.France, 10. Germany, 11.Greece, 12.India, 13.Italy, 14.Japan, 15.Mexico (New), 16.Poland, 17. Scandinavia, 18.Spain, 19.Slovinia, 20.Switzerland, 21.Turkey (New), 22.Tunisia, 23.United Kingdom, 24.Uruguay (New), 25. USA & 26.Representative from UNIDO, Austria

The commission meets annually in one of the host countries. IUE Commission 2002 meeting was held at CTC, Lyon, France during 22 - 24 April 2002 under the Chairmanship of Mr M Aloy, CTC. On super-annuation of Mr M Aloy, Dr S Rajamani, CLRI, India has been selected as the Chairman for the year 2003 onwards. Dr Jens Fennen, TFL, Switzerland is continuing as the Secretary. IUE Commission 2003 meeting was held on 29 May 2003 at Cancun, Mexico. 12 Members have attended the meeting.

The IUE has developed eleven documents relevant to the environmental protection and management.

IUE 1- Recommendations on cleaner technologies for leather production

IUE 2 - Recommendations for tannery solid by - product management

IUE 3 - Document on total dissolved solids in tannery effluent

IUE 4 - Assessment for chromium containing waste from the leather industry

IUE 5 - Typical performance for tannery waste water treatment

IUE 6 - Typical pollution values related to conventional tannery process

IUE 7 - Chargeable effluent parameters in various counties

IUE 8 - Recommendations for odour control in tannery

IUE 9 - Recommendations for sewer adapted for tannery effluents

IUE 10 - Guidelines for restricted products in leather -DRAFT

IUE 11 - Recommendations for occupational safety and health in the use of chemicals in tannery

The documents have been updated every year and few more documents are to be developed in the coming years. In addition to the development of the documents, it has been decided to widely disseminate the activities of IUE Commission with the help of organisations such as United Nations, European Commission etc. Unlike other documents the IUE document may have some legal implication so there is some constraints in the publication of IUE document. However, it has been decided to distribute the document among the interested members of all the commissions in consultation with Mr John Williams, Executive Secretary, IULTCS. Organising Regional Workshops and Seminars, publication of the IUE documents after proper editing, better interaction among IUE members are some of the planned programmes. The next IUE meeting is proposed during the first half of May 2004 at Switzerland.

3. Report of the IUF Commission - Dr C T Page
The last meeting of the IUF commission was held at BLC on Wednesday 11th September 2002. Below is a brief summary of the points discussed along with a summary of any progress since.

Draft IUF 412 - Leather - Fastness tests - Change in colour with accelerated ageing
This method was approved at the last IULTCS Delegates meeting but it was requested to expand it and include options for cycling with varying temperatures and humidities. The method was re-written and subsequently published in JSLTC for approval at the Mexico Congress Delegates meeting.

If approved this method will then be progressed as an ISO and EN method as ISO DIS 17228.

Draft IUF 452 - Leather - Tests for colour fastness - Colour fastness to crocking
This method is based on the equivalent textile methods and is specifically for leather samples. The method was published in JSLTC for approval at the Mexico Congress Delegates meeting. Following comments from the meeting, it was requested that, once approved by the Council of delegates, that this methods should be advanced as an ISO/EN method.

Updating ISO methods and consequently the equivalent IUF methods
Every 5 years the ISO methods must be reviewed by the IUF Commission (as the equivalent to the ISO Technical Committee responsible for them). All fastness methods are currently up for review. Once these have been completed and approved, it will be then appropriate to up-date the published IUF equivalents to ensure the methods are in agreement.

Reviewing old, non-ISO methods
It is a proposal to review the old IUF, but non-ISO methods, to either update them or consider their usefulness.

Publishing of IUF methods
It is noted that at least 2 of the methods sold in the SLTC binder are not according to decisions of the IUF Commission, e.g. IUF 424 is deleted and IUF 423 has the wrong title.

Summary
From the above it is clear that the program of work for the IUF is rather light in terms of new items and it is therefore good to take this period to review thoroughly what methods we already have.

Comments from those attending this Congress meeting would be appreciated with regards to additional methods considered of value to the industry. Any information related to test methods in this area would be appreciated as discussion points for the future.

4. IUP Commission - Mr J M V Williams
The last meeting of the IUP commission was held at BLC on Wednesday 11th September 2002. 8 further test methods were published in JSLTC 86, 7, December 2002, and comments were invited. Some of these methods are re-published having had alterations following the discussions since their first publication.

Most of these methods have been produced in parallel with the work of the European CEN/TC 289 Leather test methods committees and both the IU Commission members and the CEN/TC 289 committee members have had input into these published versions. Many of these methods may also be accepted as ISO standards, either in parallel vote with CEN or by a 5 month ISO vote. These will be presented to the Council of Delegates meeting for final vote and the table below shows the list of methods.

Draft IUP Number Method title Comments
IUP 3 Conditioning Revision of method approved by the Delegates meeting at the IULTCS Congress in Cape Town in March 2001
IUP 37 Measurement of water repellency of garment leathers Revision of method published in JSLTC, 86, p 81, 2002. Also required by CEN
IUP 45 Measurement of water penetration pressure Revision of method published in JSLTC, 86, p 84, 2002. Also required by CEN
IUP 46 Measurement of fogging characteristics Revision of method published in JSLTC, 86, p 73, 2002. Also required by CEN
IUP 47 Measurement of resistance to horizontal spread of flame Revision of method published in JSLTC, 86, p 77, 2002. Also required by CEN
IUP 48 Measurement of abrasion resistance of automotive leather Revision of method published in JSLTC, 86, p 79, 2002. Also required by CEN
IUP 51 Measurement of surface friction New method - IULTCS only
IUP 52 Measurement of compressibility New method - IULTCS only

NOTE: IUP 3 Conditioning. Changes to this method have been requested which include making the 23 °C/50% rh. set of conditions the default and the 20 °C/65% rh. set of conditions the alternative. Also, the conditioning time is reduced from 48 hours to 24 hours.

Draft IUP 46 - Measurement of fogging characteristics
A number of comments were received and the following amendments are required for the method:

· Section 3.5.12, 2nd line, change the word "average" to "mean value" so it reads:
….by more than 20% from the mean value for the two test pieces, ….

· Section 3.7.1, 1st line, change "sample" to "test piece," so it reads:
…for the test piece, Fv, and …..

· Section 3.7.2, use symbol F for the mean fogging value and include precision of answer required, so change to text to:
For all test pieces calculate the mean fogging value, F, in %. Report F to the nearest whole number.

· Section 4.2.1, last line of text, mistake in numbering, change 3.2.2 to 4.2.2:
….thermostatic bath (4.2.2).

· Section 4.3.2, 2nd line, clarify the meaning - current text could imply repeating the test on the same pieces! Change end of 2nd sentence to read:
…., then dry a further 2 test pieces for 7 days for the repeat test.

· Section 4.7.1, change the symbol F to G and change "means" to "mass", so the start of section 4.7.1 now reads as follows:
Calculate the mass of fogging material, Gm, and the reference mass of DOP condensed, Gdop, in milligrams using the formula:

Gm = M2 - M1

Gdop = M4 - M3

· Section 4.7.2, use symbol G for the mean mass of fogging material, so change the text to:
For all test pieces calculate the mean mass of fogging material, G, in milligrams to the nearest 0,01 mg.

· Annex A, replace the whole of Annex A with the following:

Annex A (Informative)

Inter-laboratory comparison for Method A and Method B

The results of the inter-laboratory trial reported are based on this test procedure and involved 7 laboratories, each testing 4 test specimens from the same piece of leather. 2 types of leather were tested, one a crust leather and the other a finished leather. This test data has been published in full in Leather International, August 2000.

Method A, Reflectometer method

Crust leather Finished leather
F (%) SW SV F (%) SW SV
47 9,1 16,6 74 16,4 25,1

Method B, Gravimetric method

Crust leather Finished leather
G (mg) SW SV G (mg) SW SV
3,80 0,40 0,95 7,3 0,95 1,28

SW is the standard deviation between the measurements within one laboratory and SV is the standard deviation for measurements between laboratories.

· Annex B, change the wording of the 2nd sentence in order to delete referring to "this European Standard" and "CEN".
This information is given for the convenience of the users of the method and does not constitute an endorsement of these products.

· Annex B, correct the name of equipment supplier "HAKKE" with the correct spelling "HAAKE"

2 further methods are being developed, namely, Bagginess and Soiling and these will be published in JSLTC in due course. This will complete the current programme of updating all the Physical test methods which has taken place over the last three years.

Mr Williams announced that he was retiring as Chairman of the IUP Commission and, after consulting with the members of the IUP commission, Mr C Barry Wood of BLC Leather Technology Centre Ltd, UK, would be the new Chairman. Mr Williams thanked the IUP Commission for all their support and for all their hard work over the past three years to progress so many methods.

The Commission Chairman emphasised that they welcome all Members to their meetings. Details of future meetings will be circulated to all Members and Associates. Member Association must feel free to send representatives to Commission meetings where they would be very welcome.

Almost certainly the IUC/IUF/IUP commission will continue the recent successful innovation of holding joint meetings, probably over a two day period. As many of the Commission Members sit on more than one Commission, this will save Members time and travel costs.

The next joint meeting will be communicated to all Members in due course.

The Chairman closed the meeting at approximately 1400 hrs.