Protocol Page 1 of 11. Protocol for Proficiency testing scheme for Bitumen Programme No. GPTS/PT 05
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1 Tel Nos , , Mob Nos , , Fax Nos Protocol Page 1 of 11 Protocol for Proficiency testing scheme for B 2, Basement, Samudra Complex, Nr. Hotel Klassic Gold, Off. C.G. Road, Sardar Tel Nos , , Cell Nos , , Fax Nos , E mail sales@globalptservices.com, nilesh@globalptservices.com Web Records of Revision status and Modifications Revision Revision Date Details Authorized by
2 Tel Nos , , Mob Nos , , Fax Nos Proficiency testing scheme for Protocol Page 2 of 11 Index No. Content Page 1.0 Profile Background Programme details Quality Control Features Non conforming products Technical Information Sample Selection, Homogenization and sample preparation Sample Packaging and Delivery Sample Testing Reporting the results Choice of methodology Removal of errors and blunders Number of permitted results Performance Evaluation Collusion and falsification of results Analysis of Results Approaches to data analysis Setting assigned values Calculating z scores Standard deviation for proficiency assessment (SDPA) Interpreting results Confidentiality Statement Report Feedback Registration for participation Time line Participation fee Contact details of PT Co ordinator 11
3 1.0 Profile 1.1 Background Tel Nos , , Mob Nos , , Fax Nos Protocol Page 3 of 11 GPTS is the apex body providing proficiency testing services to the NABL accredited testing laboratories in the Chemical discipline (NABL 103, Specific guidelines for chemical testing laboratories) and Mechanical discipline (NABL 107, Specific guidelines for mechanical testing laboratories). The PT programmes initiated for the year are for the, cement, and waste water. These schemes are to be conducted independently. 1.2 Programme details GPTS is now launching PT scheme on testing of (). The study is being coordinated by Nilesh Padhariya. The programme envisages testing of homogenized sample of as per Indian Standard (Standard test methods for analysis of bitumen) of testing. Minimum 20 laboratories are expected to participate. The registration for participation would be done on first come first served basis. The programme would be conducted as per ISO 17043:2010. The channel of communication with all the participants will remain open throughout the programme implementation period through e mail / telephonic communication / letter. All participant labs are required to submit the results of test on or before specified date given on web site / protocol, whichever is earlier. Proficiency test item is prepared from the single source by sample preparation methods based on Indian Standards, and is carefully selected to meet the need of participants. Wherever practical, Proficiency test item will be as similar as possible to those samples routinely tested by participating laboratories. However, in some cases, in order to achieve the required degree of homogeneity and stability, Proficiency test item may be in the form of simulated samples. The range of Proficiency test item will usually be varied from round to round in order to be realistic and challenging. Details of individual Proficiency test item are available in the scheme description for each scheme. 1.3 Quality Control A number of factors will be taken into consideration when determining the quality control testing required to be performed on each type of proficiency test item. These include the degree of natural homogeneity, the stability of the proficiency test item, and the use of process control during production. Where undertaken, homogeneity assessment is carried out based on the procedure described in the ISO Further details regarding homogeneity testing are included in the scheme descriptions and/or reports.
4 Tel Nos , , Mob Nos , , Fax Nos Proficiency testing scheme for Protocol Page 4 of 11 For some schemes, for certain circumstances, homogeneity may not be undertaken on every proficiency test item type prior to despatch. This may be for operational reasons, or where the process has been proven to provide homogeneous samples. In these instances the participants results are used to assess sample homogeneity and any issues will be treated as described below for non conforming products. 1.4 Features Each participating laboratory will be provided proficiency test item for testing. Features of the scheme are as below; Homogenization of sample and its preparation, Conducting the checks on homogeneity and statistical check for homogeneity, Safe delivery of samples to participating laboratories, by selecting the appropriate courier / transporter depending on the size (Approx. 5 Kgs.) of the proficiency test item,, Analysis of Data as per ISO 17043:2010 and ISO 13528:2005, Reporting feedback of performance to all participants individually by detail report alongwith the lab no. for identification of their performance, and Maintaining confidentiality of data analysed during the course of programme All the participants will be co ordinated by GPTS. Activities like material homogenization and checks on homogeneity will be subcontracted by GPTS to other NABL Accredited Laboratories from the Approved Subcontractor List. In case of noticeable variation is observed in homogeneity, than the government laboratory may be consulted at National Level and will be considered as final. Activities like statistical check of homogeneity, compilation, and analysis of results and report preparation will be done by GPTS. All such information will be made strictly confidential during the implementation of the scheme 1.5 Non conforming products Where, prior to dispatch, the homogeneity and/or the stability of proficiency test items are not accepted, the proficiency test items will be withdrawn prior to distribution to participants. Where this may cause a delay in the distribution of proficiency test items, participants will be informed. Occasionally, issues with proficiency test item may not be identified until after distribution. Under these circumstances, this is taken into account when assessing participant results. The outcome will vary depending upon the situation but may involve reporting of performance scores for information only, or the provision of replacement proficiency test items. In these instances, full details will be provided to participants.
5 Tel Nos , , Mob Nos , , Fax Nos Proficiency testing scheme for Protocol Page 5 of Technical information 2.1 Sample Selection, Homogenization and sample preparation The sample will be homogenized and evaluated statistically for homogeneity. The material will also be checked for its stability. Stability check will be conducted around the actual date of testing by the participants we are homogeneity and stability checks as per ISO Annex B. The data from a homogeneity check are represented by; x t, k where, t represents the sample (t = 1, 2..., g) k represents the test portion (k = 1, 2) Define the sample averages as: xt,. = (xt,1 + xt,2) / 2 and the between test portion ranges as: w t = Ix t,1 x t,2i Calculate the general average; x. r = x t / g The standard deviation of sample averages; S x = (xt x) 2 / (g 1) and the within samples standard deviation: S w = wt 2 / (2g) Where the summations are over samples (t = 1, 2,..., g). Finally, calculate the between samples standard deviation as: S s = S x 2 (S w 2 / 2) Accepted Limit S s 0.3 x SDPA Assessment criterion for a stability check ABS (x y) 0.3 x SDPA Where, x = General average of the measurements obtained in the homogeneity check. y = General average of the results obtained in the stability check.
6 2.2 Sample Packaging and Delivery Tel Nos , , Mob Nos , , Fax Nos Protocol Page 6 of 11 The prepared PT item / proficiency test items would be taken from the homogenized lot(s) and packed properly and safely, for dispatch to the participants. Each participating laboratory would be provided proficiency test item. Necessary instruction and results reporting sheets will also be provided. Replacement may be provided in case of damage or loss during transit, after verification of the condition of the sample. All such samples will be sent by reputed transporters and will try for the door delivery basis. However in case of odd locations, if transporter is not willing to deliver on door to door basis, in that case participant laboratory is requested to collect the sample from the transporter s godown. For the local laboratories within the Ahmedabad, we may provide hand delivery services to the laboratory. Proficiency test items are sent in appropriate packaging and under conditions intended to maintain the integrity of the proficiency test items during transit. Once packages have been delivered, cannot be held responsible if they subsequently fail to reach the correct personnel or are not stored under the recommended conditions. Participants are asked to check the contents of package immediately on receipt and to contact, if there are any problems with the condition of the proficiency test item or accompanying documentation. If packages are received damaged, then it would be very useful, if participants could supply photographic evidence to assist our investigations 2.3 Sample Testing The schemes cover testing of homogenized samples as per the relevant Indian standard (Standard test methods for analysis of bitumen) for the following parameters; Sr. No. Test parameter Expected Range Relevant test standards 1. Specific gravity 0.99 to 1.10 IS 1202:1978 Reaffirmed Penetration 60 to 70 mm IS 1203:1978 Reaffirmed Softening point 50 to 55 C IS 1205:1978 Reaffirmed Ductility 80 to 100 cm IS 1208:1978 Reaffirmed 2009 Participant laboratories are required to ensure availability of calibrated equipment and required environmental conditions, and meet all the requirements of Indian standard (Standard test methods for analysis of bitumen) during testing. Participant laboratories have to ensure compliance with the relevant test standards, such as Indian Standard (Standard test methods for analysis of bitumen).
7 2.4 Reporting the results Tel Nos , , Mob Nos , , Fax Nos Protocol Page 7 of 11 Participant laboratories are required to conduct the number of tests as required in the relevant Indian Standard (Standard test methods for analysis of bitumen) and report the result for each sample, to the accuracy mentioned; deviation, if any. All such information needs to be reported in the result sheet given as Annex A (F/OPN/03). Test results must be sent to the coordinator through e mail / fax for quick transmission, followed by hard copy. All such results should be suitably typed in the result sheet and also all participant laboratories are requested to submit hand written data gathered during the performance of test for the verification purpose. Result sheet and raw data sheet must be approved by Authorized Signatory of the participant laboratory by signing the reports alongwith the clear identification of name of the person authorizing the report and seal of participant laboratory. It is recommended that results and calculations are checked thoroughly before reporting. Results should be reported clearly, in the format and these details in the Scheme Description. If calculations are used, unless instructed otherwise, the laboratory is to report only the final calculated result. Part of the challenge of Proficiency testing is the ability to perform calculation and transcribe results correctly. staff cannot interpret or calculate results on participants behalf. Once submitted and received, results cannot be amended and no changes can be made after the report has been issued. In general, results of zero should not be reported; results should be reported depending upon the detection limit of the method used, for example, <10. The exception is a small number of parameters, where it may be appropriate to report a result of zero, depending on the measurement scale being used. Results of zero and truncated results, such as <or> cannot be included in the data analysis and therefore cannot be allocated a numerical performance score. Results may be rounded up or down for the purpose of reporting and may not therefore be identical to your original reported result. The effects of rounding may also mean that occasionally percentage totals do not add up exactly to 100%. 2.5 Choice of methodology Participants are expected to use the test method given in this protocol; however they may choose technically appropriate test or measurement procedures of their choice unless otherwise instructed. Participants are asked to treat the proficiency test items as a routine sample as much as possible.
8 2.6 Removal of errors and blunders Tel Nos , , Mob Nos , , Fax Nos Protocol Page 8 of 11 Although robust estimators are used in order to minimize the influence of outlying results, extreme results or results that are identifiable invalid should not be included in the statistical analysis of the data. For example, these may be results caused by calculation errors or the use of incorrect units. However, such results can be difficult to identify by the PT or the use of incorrect units. However, such results can be difficult to identify by the PT organizer. For this reason, the robust average and standard deviation will be calculated but those results that are out of the assigned value ± 6 x SDPA will be excluded and the robust average and standard deviation will then be re calculated. These re calculated values will be used for the statistical analysis. All results, including excluded results, will be given performance scores. 2.7 Number of permitted results Although it is desirable for participants to submit multiple results in order to compare results between different analysts, methods or instruments, a single laboratory reporting a large number of results could potentially bias the dataset. In order to minimize the effects of bias, GPTS therefore limits the number of results participants are able to report. However during analysis, the GPTS will do averaging of all such results and then it will be taken for analysis. 2.8 Performance Evaluation Performance score will be evaluated in terms of z/z score as per the ISO Collusion and falsification of results If defeats the objective of taking part in proficiency testing of participants are not returning genuine results. Certain measures are built into the scheme to try to prevent collusion, for example, assigned values are not made known to anyone before the report is issued and no results are accepted after the publication of the report. Participants will be contacted, if there is clear evidence of collusion. However, ultimately the responsibility rests with each participant to behave in a professional manner.
9 3.0 Analysis of Results 3.1 Approaches to data analysis Tel Nos , , Mob Nos , , Fax Nos Protocol Page 9 of 11 Different approaches to data analysis may therefore be used, the most common approaches being described below. Further information on the statistical approach for specific schemes is also provided in the scheme descriptions and scheme reports. The advantages of using a perform score are: Results can be expressed in a form that is relatively easy to interpret and understand Results can be summarized in graphical or tabular form to depict overall performance A performance score allows participants to directly compare their own result with others If consistent statistical values are applied, a performance score enables participants to monitor and trend their own performance over time. When reviewing results, participants should take into account the methods used to analyse the data and to assess performance, and should review their performance in context, taking into account performance of the whole dataset. 3.2 Setting assigned values The assigned value is the value selected as being the best estimate of the true value for the parameter under test. For quantitative tests, all assigned values are derived in accordance with ISO The assigned value is determined from the consensus value of participants results, or from expert laboratories, robust statistical methods are used for calculation of the consensus value, details 3.3 Calculating z scores z score = (x X) / SDPA Where; x = the result reported by the participant X = the assigned value SDPA = Standard Deviation for Proficiency Assessment The z score expresses performance in relation to an acceptable variation of the participant result to the assigned value. 3.4 Standard deviation for proficiency assessment (SDPA) The method used to determine the SDPA derived in accordance with ISO SDPA is determined from the dispersion of participant results, robust statistical methods are used for the standard deviation, This fixed value may be absolute or expressed as a percentage of the assigned value.
10 3.5 Interpreting results Tel Nos , , Mob Nos , , Fax Nos Protocol Page 10 of 11 Laboratories reporting the assigned result or range of results will be considered correct, and therefore have satisfactory performance. For the following interpretation is given to z scores results. z 2.00 Satisfactory result 2.00 < z <3.00 Questionable result z 3.00 Unsatisfactory result Where other performance techniques are used theses are described in the Scheme Description and/or report. For small data sets (generally with less than 8 results) there will be increased uncertainty around the assigned value, were consensus values from participants results. For those analytes that use a formulation or reference value as the assigned value and a fixed fit for purpose SDPA (see 5.6 of ISO 13528) z scores will be provided. Where the assigned value and/or SDPA are based on participant results, performance scores will be given for information only. For data sets with very limited results or where the spread of results is large, z scores may not be provided with regards to where a z score may be provided rather than a z score. 3.6 Confidentiality Statement All laboratories will be given unique code number and that code number will be fixed through out the proficiency testing scheme. The other participants does not have access to the code number and by that way the confidentiality is maintained through out the proficiency testing scheme. Analysed data, laboratory results sheet, laboratory name, and feedback will be made strictly confidential. However, it may be disclosed to NABL / Accreditation body, if required. It is also made available to NABL Assessor during our assessment by NABL. 3.7 Report Report will be released in two stage as below upon completion of the analysis of data of all participants as per the method described above; Participant wise individual letter will be prepared and the performance of the participants will be delivered in the letter and is called draft report, Later on full and compiled report will be prepared having all the statistics, graphs etc. containing details of the programme, evaluation, laboratory performance will be prepared and sent to all participants. Copy of the detail report may be given to NABL / Accreditation body, if required. This is called final report, which may be released later after release of draft report.
11 3.8 Feedback Tel Nos , , Mob Nos , , Fax Nos Protocol Page 11 of 11 Participant laboratories will be conveyed the status of their performance, with remarks to monitor / improve their performance. The criteria for evaluation of performance will be identified in the report for ease of understanding by the participant laboratories. 4.0 Registration for participation Participant laboratories having facilities for testing of bitumen can register by providing the required information in the form no. 1 submitted alongwith the introductory letter, for their participation. 5.0 Time line The last date for registration in the scheme is 31 st July Proficiency test items would be delivered to participants laboratories in 2 nd Week of August Effort will be made to ensure that all participant laboratories will get the sample on or before 3 th Week of August All participant laboratories are requested to start testing of the sample and will complete all tests by 7 th September All participant laboratories have to submit the results of test latest by 7 th September Final detail analysis report will be submitted to all participant laboratories latest by 15 th September 2015 for their performance on proficiency testing. 6.0 Participation fee Rs. 12, 000/ plus service tax 7.0 Contact details of PT Co ordinator Mr. Nilesh Padhariya Chief Executive Officer Patel Nagar, Ahmedabad , Gujarat, India Tel Nos , , Cell Nos , , Fax Nos , E mail sales@globalptservices.com, nilesh@globalptservices.com Web
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