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AFRIMETS – AFM Pilot Study Final Report 1 AFRIMETS Secretariat Private Bag X34 Lynnwood Ridge 0040 AFRIMETS - AFM Pilot Study Final Report Giza, Egypt, September 2014

AFRIMETS - AFM Pilot Study Final Report Groups/Mass/SiteAssets...The measurement results were sent to the AFM in a final report. A list of the equipment used as balances and environmental

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Page 1: AFRIMETS - AFM Pilot Study Final Report Groups/Mass/SiteAssets...The measurement results were sent to the AFM in a final report. A list of the equipment used as balances and environmental

AFRIMETS – AFM Pilot Study Final Report

1

AFRIMETS Secretariat Private Bag X34 Lynnwood Ridge 0040

AFRIMETS - AFM

Pilot Study

Final Report

Giza, Egypt, September 2014

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Contents Abstract 1. Introduction .......................................................................................... 3 2. Aim of the Programme ......................................................................... 4 3. Participants ........................................................................................... 4 4. Design of the Programme ..................................................................... 5 5. Reporting ............................................................................................... 6 6. Stability of the travelling standards .................................................... 6 7. Reference Values ................................................................................. 6 8. Results and Discussion ...................................................................... 6 9. Conclusions ......................................................................................... 6 10. References ................................... ................................... 7

Annex I ……………………………………… ………………………… 8

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Abstract:

A round robin Supplementary Mass comparison Programme between NMIs of Arab countries (Egypt, Iraq, Syria, Jordan and Tunisia) in addition to the NMI of South Africa (NMISA) was carried out during the period of November 2011 to April 2013. The AFM identification number for this comparison was: ARABMET M.S.1. The mass department of the National Institute for Standards (NIS) of Egypt accepted to play the role of Pivot Lab and provided one set of weights with nominal values: 1 kg, 500 g, 2 g, and 100 mg. The set was circulated among the participating NMIs. The procedures and instructions are given according to the INTERNATIONAL RECOMMENDATION OIML R 111-1 Edition 2004 (E) [1]. This comparison was registered in the BIPM KCDB in June 2012 as an AFRIMETS supplementary comparison under the identifier AFRIMETS.M.M-S2. With NIS withdrawing from M.M-S2, and the member from Tunisia that is not a designated institute leaving NMISA as the only one AFRIMETS member of the BIPM in the comparison, it therefore became very difficult to keep it as an AFRIMETS supplementary comparison. To make use of the efforts made by participants and the organizers of the programme it was decided to issue the report as the result of a Pilot Study. Such a report can still be used by the AFM member NMIs as supporting evidence for CMCs. The results obtained are represented in this report. The analysis of the results and final report has been done by AFM technical support unit. 1- Introduction:

The technical Support Unit (TSU) of the Arab Federation for Metrology (AFM) developed a questionnaire to assist the Arab Metrology Programme ARABMET to develop appropriate protocols and schedules for an intended intercomparisons schemes. In 17 / 5 / 2011 the TSU distributed the questionnaire among Arab Metrology Institutions. Positive response was received from 5 Arab NMIs requesting the participation in two fields, namely Length and Mass Measurements. The comparison programme proposed was of the Round Robin type. It was then decided that the Arab Federation for Metrology (AFM) would extend its invitation to the National Metrology Institutes (NMIs) to participate in measurement comparison program in the prescribed metrological fields. The comparison programms were designed, organized and coordinated by AFM Technical Support Unit (TSU) under technical support of the National Institute for Standards (NIS) of Egypt being an active member of both the Programme and the Federation at the time. The comparison program was open for NMIs of the members and non members Arab states of the Federation. The comparisons were to be conducted following appropriate measurement protocols. The objectives of the comparison programmes are to provide the participating laboratories with means for comparing their measurement results, opportunities for technical capability improvements and recognition of Calibration and Measurements Capabilities (CMCs). AFM, being an observer member of the Intra-Africa Metrology System (AFRIMETS), worked through concerned AFRIMETS authorities to submit the comparison programmes for registration as AFRIMETS supplementary comparisons on the BIPM KCDB. Thus, the National Metrology Institute of South Africa (NMISA) has been invited to join the round robin scheme. One set of weights, with nominal values 100 mg, 2 g, 20 g, 500 g and 1 kg is chosen as the artifacts for the comparison. All of the weights are made of non-magnetic stainless steel. The Mass laboratory of NIS- Egypt accepted to provide the travelling standards, the comparison protocol and the reference values of the standards under comparison. The measurements in this comparison were carried out from November 2011 to April 2013. The measurements were carried out according to a protocol approved by the concerned Regional Metrology Organization technical authorities, namely AFRIMETS and endorsed by the Consultative Committee for Mass and Related Quantities (CCM)

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NIS Mass Lab. opted not to continue acting as a pilot lab and asked, through NIS top management, to withdraw from the programme on the 24th of November 2013, 6 months after submitting their results of the last measurement of the round. The AFRIMETS TC-Mass decided to withdraw AFRIMETS.M.M-S2 from the official list of AFRIMETS comparisons. The Chair of TC-Mass, who happened to be the Head of NIS mass lab, then, informed CC-Mass that the comparison will not be completed as a supplementary and should be removed from the KCDB list. Due to the withdrawal of NIS, unfortunately it cannot be called an AFRIMETS Supplementary comparison anymore and it is renamed AFRIMETS-AFM Pilot Study. It cannot be published in the KCDB but can be used as supporting evidence for CMC claims. It is advised that, probably, it should be followed by a second participation or a bilateral comparison once they want to submit CMCs. As NIS Mass laboratory opted lately not to act as the pivot lab, the measurement results obtained are evaluated by AFM TSU and reported to the participating laboratories by the programme coordinator. 2- Aim of the Programme:

The aim of this comparison is to give confidence in the technical capacity of the AFM members and non members as a step towards the publication of CMCs in the BIPM KCDB to gain international Statement of Equivalence in accordance with the mutual recognition agreement (CIPM – MRA). The participation of NMISA – South Africa helped in achieving these goals through its active participation in Sub Regional Metrology Organizations (SRMOs) members of AFRIMETS. The comparison gives objective evidence on the technical competence of laboratories participated, and it assists in identifying opportunities to improve the metrological capacity of those Laboratories.

3- Participants:

Table 1 shows the participating NMIs, their affiliations and the planned time schedule.

No. Country - Laboratory -

Abbreviation Date Planned Metrology region

1* EGYPT - National Institute of Standards – NIS*

November 2011 December 2011

Pilot Lab*; AFM Member, AFRIMETS Member (NEWMET), APMP Associate Member and EURAMET Corresponding Member

2 IRAQ - Central Organisation

for Standardisation and Quality Control - COSQC

January 2012 February 2012

AFM Member

3 SYRIA - National Standards and Calibration Laboratory -

NSCL

March 2012 April 2012

AFM Member APMP Associate Member

4 SOUTH AFRICA - National Metrology Institute of South

Africa - NMISA

May 2012 June 2012

Invited Lab. – AFRIMETS Member (SADCMET); APMP Associate Member

5

TUNISIA - Central Laboratory for Testing and

Analysis-Metrology Center - LCAE-CME

July 2012 August 2012

AFRIMETS Member (MAGMET)

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6 JORDAN - Jordan National Metrology Institute - JNMI

September 2012 October 2012

AFM Member

1* EGYPT - National Institute of Standards – NIS*

November 2012 December 2012

Pilot Lab*; AFM Member, AFRIMETS Member (NEWMET) and EURAMET Corresponding Member

* NIS Mass Lab. opted not to continue acting as a pilot lab and asked, through NIS

top management, to withdraw from the programme on the 24th of November 2013, 6 months after submitting their results of the last measurement of the round.

4- Design of the Programme:

The program was designed according to the guidelines for CIPM (Comité International des Poids et Measures) key comparisons [2]. Five travelling standards of 1 kg, 500 g, 20 g, 2 g and 100 mg were used in accordance with the International Recommendation OIML R111 [1]. The travelling standards were circulated between the participants as shown in table 2. As pilot laboratory, NIS- Egypt should determine the conventional mass of the travelling standards at the beginning and the end of the comparison. As NIS Mass laboratory opted, after the end of the programme, not to act as the pilot lab regarding the analysis of the results reported by the participants, the measurement results obtained are evaluated by AFM TSU and reported to the participating laboratories by the programme coordinator. The transportation sequence and measurements of the travelling standards has been done as shown in figure 1. The measurements were conducted starting in November 2011 at NIS mass lab. Then the artifact moved to Institute number 2 and so on. No significant accident has been reported during the comparison. However, the artifacts stayed for a longer period than planned at JNMI waiting for the measurement standard to be calibrated to ensure traceability to SI units.

Serial NMI - Country Artefact Received Report Delivered 1 NIS - Egypt November 2011 28 March 2012 2 COSQC - Iraq 14 December 2011 11 January 2012 3 NSCL - Syria 21 January 2012 10 April 2012 4 NMISA - South Africa 15 March 2012 27 June 2103 5 LCAE - Tunis 28 June 2012 28 April 2013 4 JNMI - Jordan 2 October 2012 13 March 2013 7 NIS - Egypt 30 March 2013 15 April 2013

Table 2:- Sequence of the measurements

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Figure (1) shows the transportation sequence and measurements of the travelling standards. 5- Reporting:

The measurement results were sent to the AFM in a final report. A list of the equipment used as balances and environmental conditions, details of measurement procedure and uncertainty analysis were included and the reference standard used in order to see the traceability at each laboratory. 6- Stability of the travelling standards: NIS mass Lab, as the pilot lab, did not provide any data regarding the stability of the travelling standard neither at the start of the round nor with the results at the end of the measurements round!!

A statement on the stability was thought to be necessary to ensure that the conventional mass values of the traveling standards were stable during the measurements period. The travelling standards were circulated among the five participating laboratories without any incident that required any return to the pilot laboratory to re-measure the travelling standards. 7- Reference values

NIS Mass lab did not provide any information regarding the Reference Value or any Statement on density determination. NMISA agreed to provide the reference value instead of NIS-Egypt. The normalized error value En is obtained from the following expression.

/

Where En is the normalized error

NIS‐Egypt

NSCL ‐Syria

JNMI ‐Jordan

LCAE ‐Tunis

NMISA ‐South Africa

COSQC ‐Iraq

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ml is the lab. Value mref is the reference value Ucl is the combined uncertainty of the lab. Ucref is the combined uncertainty of the reference lab.

8- Results and discussions:

The results of the inter-comparison have been presented in graphs and tables “Annex I” showing the true and conventional mass of the weights with their uncertainties as provided by participant laboratories. The results show a good agreement in the measurements between the participants; however the results of the labs could not be compared with the reference value that was supposed to be delivered by NIS- Egypt. NIS did not provide NIS results in accordance with the agreed protocol formats neither at the beginning nor at the end of the programme. Furthermore, NIS Mass Lab, supported by NIS top Management asked to withdraw from the programme after six months from delivering its measurement results at the end of the round. Hence it was decided not to work with NIS reference value and to exclude its results from the report.

9 – Conclusions:

First mass inter comparison between ARABMET members has been successfully completed.

Measurements reports provided by participants show a well established scientific discipline in mass metrology in the participant laboratories.

Data Equipment, procedures followed and traceability listed in the participants reports show a very good infra- structure for mass metrology in the participant laboratories.

The inter-caparison programme assures the ability of the participant laboratories to provide a world class results in mass metrology.

10- References

1. INTERNATIONAL RECOMMENDATION OIML R 111-1 Edition 2004 (E) “Weights of classes E1, E2, F1, F2, M1, M1–2, M2, M2–3 and M3 Part 1: Metrological and technical requirements”

2. CCM – AFRIMETS - ARABMET Mass Supplementary Inter-comparison AFRIMETS.M.S1 Instructions and Technical Protocol.

3. Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement Results

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4. W. Wöger, “Remarks on the En-criterion Used in Measurement Comparison,

Internationale Zusammenarbeit.PTB-Metteilungen 1999.Pages 24-27

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Annex I Table (1) the measured values and the Uc of participant laboratories for 1 kg (k=2)

Institute Name  Measured value (g)  Uc (mg) 

NSCL 1000.00267 0.25400

COSQC 1000.0007 0.14466

JNMI 1000.002544 0.50000

LCAE-CME 1000.00056 0.15000

NMISA 1000.002439 0.02627

True Mass

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Table (2) the measured value and the Uc of participant laboratories for 500 g (k=2)

Institute Name  Measured value (g)  Uc (mg) 

NSCL 500.00073 0.12300

COSQC 500.0000012 0.18093

JNMI 500.000439 0.25000

LCAE-CME 500.000291 0.08000

NMISA 500.0004129 0.02310

True Mass

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Table (3) the measured value and the Uc of participant laboratories for 20 g (k=2)

Institute Name  Measured value (g)  Uc (mg) 

NSCL 19.251 0.01200

COSQC 20.0000676 0.05116

JNMI 20.0000408 0.02500

LCAE-CME 20.0000184 0.00800

NMISA 20.000029 0.00289

True Mass

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Table (4) the measured value and the Uc of participant laboratories for 2 g (k=2)

Institute Name  Measured value (g)  Uc (mg) 

NSCL 2.00028 0.00600

COSQC 2.0000358 0.02545

JNMI 2.000047895 0.01200

LCAE-CME 2.0000495 0.00400

NMISA 2.00005 0.00118

True Mass

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Table (5) the measured value and the Uc of participant laboratories for 100 mg (k=2)

Institute Name  Measured value (g)  Uc (mg) 

NSCL 0.100023 0.00300

COSQC 0.100000618 0.02355

JNMI 0.10001967 0.00500

LCAE-CME 0.100022 0.00150

NMISA 0.100023 0.00108

True Mass

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Figure (1) shows the true mass of the participants results for 1 kg, and uncertainty (k=2)

0.00

0.50

1.00

1.50

2.00

2.50

3.00

3.50NSCL

COSQ

C

JNMI

LCAE‐CME

NMISA

(M‐M

nominal )/m

g

Laboratory

1 kg True Mass

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Figure (2) shows the true mass of the participants results for 500 g, and uncertainty (k=2)

‐0.40

‐0.20

0.00

0.20

0.40

0.60

0.80

1.00

NSCL

COSQ

C

JNMI

LCAE‐CME

NMISA

(M‐M

nominal )/m

g

Laboratory

500 g True Mass

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Figure (3) shows the true mass of the participants results for 20 g, and uncertainty (k=2)

0.00

0.02

0.04

0.06

0.08

0.10

0.12

0.14

NSCL

COSQ

C

JNMI

LCAE‐CME

NMISA

(M‐M

nominal )/m

g

Laboratory

20 g True Mass

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Figure (4) shows the true mass of the participants results for 2 g, and uncertainty (k=2)

0.00

0.01

0.02

0.03

0.04

0.05

0.06

0.07

NSCL

COSQ

C

JNMI

LCAE‐CME

NMISA

(M‐M

nominal )/m

g

Laboratory

2 g True Mass

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Figure (5) shows the true mass of the participants results for 100 mg, and uncertainty (k=2)

‐0.01

0.00

0.01

0.01

0.02

0.02

0.03

0.03

NSCL

COSQ

C

JNMI

LCAE‐CME

NMISA

(M‐M

nominal )/m

g

Laboratory

100mg  True Mass

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Table (6): Difference in assigned values between laboratory A and laboratory B for true mass of 1kg; Δm (mg).

 NSCL COSQC JNMI LCAE-CME NMISA

        

NSCL    0.00197  0.000126  0.00211  0.000231 

COSQC ‐0.00197     ‐0.001844  0.00014  ‐0.001739 

JNMI ‐0.000126  0.001844     0.001984  0.000105 

LCAE-CME ‐0.00211  ‐0.00014  ‐0.001984     ‐0.001879 

NMISA ‐0.000231  0.001739  ‐0.000105  0.001879    

              

Table (7): Difference in assigned values between laboratory A and laboratory B for true mass of 500g; Δm (mg).

 NSCL COSQC JNMI LCAE-CME NMISA

        

NSCL    0.000353  0.000094  0.000242  0.0001201 

COSQC ‐0.000353     ‐0.000259  ‐0.000111  ‐0.0002329 

JNMI ‐0.000094  0.000259     0.000148  0.000261 

LCAE-CME ‐0.000242  0.000111  ‐0.000148     ‐0.0001219 

NMISA ‐0.0001201  0.0002329 ‐2.61E‐05  0.0001219    

              

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Table (8): Difference in assigned values between laboratory A and laboratory B for true mass of 20g; Δm (mg).

 NSCL COSQC JNMI LCAE-CME NMISA

        

NSCL    ‐1.96E‐05  7.2E‐06  2.96E‐05  1.9E‐05 

COSQC 1.96E‐05     2.68E‐05  4.92E‐05  3.86E‐05 

JNMI ‐7.2E‐06 ‐2.68E‐05 2.24E‐05 1.18E‐05

LCAE-CME ‐2.96E‐05  ‐4.92E‐05  ‐2.24E‐05     ‐1.06E‐05 

NMISA ‐1.9E‐05 ‐3.86E‐05 ‐1.18E‐05  1.06E‐05

              

Table (9): Difference in assigned values between laboratory A and laboratory B for true mass of 2g; Δm (mg).

 NSCL COSQC JNMI LCAE-CME NMISA

        

NSCL 1.2E‐05 2.105E‐06  5E‐07 0

COSQC ‐1.2E‐05     ‐9.895E‐06  ‐1.15E‐05  ‐1.2E‐05 

JNMI ‐2.105E‐06  9.895E‐06     ‐1.605E‐06  ‐2.105E‐06 

LCAE-CME ‐5E‐07  1.15E‐05  1.605E‐06     ‐5E‐07 

NMISA 0  1.2E‐05  2.105E‐06  5E‐07    

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Table (10): Difference in assigned values between laboratory A and laboratory B for true mass of 100mg; Δm (mg).

 NSCL COSQC JNMI LCAE-CME NMISA

        

NSCL    2.28E‐05  3.33E‐06  1E‐06  0 

COSQC ‐2.28E‐05     ‐1.947E‐05  ‐2.18E‐05  ‐2.28E‐05 

JNMI ‐3.33E‐06  1.947E‐05     ‐2.33E‐06  ‐3.33E‐06 

LCAE-CME ‐1E‐06  2.18E‐05  2.33E‐06     ‐1E‐06 

NMISA 0  2.28E‐05  3.33E‐06  1E‐06    

              

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The En value for the measurement results for 1kg taking the result of NMISA as the reference value Ref. value of NMISA (M) –Nominal (Mn) = 0.002439 g

Institute Name  Lab value M Inst. 

(MI)‐Mn (g) 

Uc  (mg) 

En 

  

NSCL 0.00267 0.25400 0.9046234 

COSQC 0.0007 0.40000 ‐4.338154 

JNMI 0.002544 0.50000 0.2097108 

LCAE-CME 0.00056 0.15000 ‐12.33887 

NMISA 0.002439 0.02627 0 

  

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‐14.00

‐12.00

‐10.00

‐8.00

‐6.00

‐4.00

‐2.00

0.00

2.00

En‐value

Laboratory

En‐Value for 1kg

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The En value for the measurement results for 500 g taking the result of NMISA as the reference value Ref. value of NMISA (M) –Nominal (Mn) = 0.4129 g  

Institute Lab. Name  

Lab value Ml‐Mn  (g) 

Uc (mg) 

En 

  

NSCL 0.000533 0.12300 0.959646 

COSQC 0.0001800 0.23000 ‐1.008 

JNMI 0.000439 0.25000 0.1040 

LCAE-CME 0.000291 0.08000 ‐1.4639 

NMISA 0.0004129 0.02310 0 

  

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‐2.00

‐1.50

‐1.00

‐0.50

0.00

0.50

1.00

1.50

(En‐value

Laboratory

En‐value for 500 g 

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The En value for the measurement results for 20 g taking the result of NMISA as the reference Ref. value of NMISA (M) –Nominal (Mn) = 2.9E-05 g

Institute Name  Lab value Ml‐Mn 

(g) Uc (mg) 

En 

  

NSCL 0.0000480 0.01200 1.539322 

COSQC 0.0000676 0.01000 3.708247 

JNMI 4.08E-05 0.02500 0.468878 

LCAE-CME 1.84E-05 0.00800 ‐1.24618 

NMISA 2.9E-05 0.00289 0 

  

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‐2.00

‐1.00

0.00

1.00

2.00

3.00

4.00(En‐value

Laboratory

En‐value for 20 g 

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The En value for the measurement results for 2 g taking the result of NMISA as the reference Ref. value of NMISA (M) –Nominal (Mn) = 5E-05 g

Institute Name  Lab value Ml‐Mn 

(g) Uc (mg) 

En 

  

NSCL 5E-05 0.00600 0 

COSQC 0.0000380 0.00345 ‐3.29108 

JNMI 4.7895E-05 0.01200 ‐0.17457 

LCAE-CME 4.95E-05 0.00400 ‐0.11989 

NMISA 5E-05 0.00118 0 

  

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‐3.50

‐3.00

‐2.50

‐2.00

‐1.50

‐1.00

‐0.50

0.00

0.50(En‐value

Laboratory

En‐value for 2 g 

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The En value for the measurement results for 100 mg taking the result of NMISA as the reference Ref. value of NMISA (M) –Nominal (Mn) = 2.3E-05 g

Institute Name  Lab value Ml‐Mn 

(g) 

Uc (mg) 

En 

  

NSCL 2.3E-05 0.00300 0.0000 

COSQC 0.0000002 0.00100 ‐15.4905 

JNMI 1.967E-05 0.00500 ‐0.65099 

LCAE-CME 2.2E-05 0.00150 ‐0.54102 

NMISA 2.3E-05 0.00108 0.0000 

  

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AFRIMETS – AFM Pilot Study Final Report

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‐18.00

‐16.00

‐14.00

‐12.00

‐10.00

‐8.00

‐6.00

‐4.00

‐2.00

0.00

2.00

(En‐value

Laboratory

En‐value for 100 mg