NISTIR 7880-32 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1992 

Comparability Studies 

Results for Round Robins XXIV, XXV, and XXVI 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 3 Ascorbic Acid in Human Serum 

Neal E. Craft (Former Employee) 

David L. Duewer 

Margaret C. Kline 

Sam A. Margolis (Retired) 

Willie E. May 

Katherine E. Sharpless 

Jeanice B. Thomas 

This publication is available free of charge from 

http://dx.doi.org/10.6028/NIST.IR.7880-32 

 

 

 

 

NISTIR 7880-32 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1992 

Comparability Studies 

Results for Round Robins XXIV, XXV, and XXVI 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 3 Ascorbic Acid in Human Serum 

Neal E. Craft (Former Employee)
 

David L. Duewer
 

Sam A. Margolis (Retired)
 

Jeanice B. Thomas
 

Chemical Sciences Division, Materials Measurement Laboratory 

Margaret C. Kline 

Biomolecular Measurement Division, Materials Measurement Laboratory 

Katherine E. Sharpless 

Office of Special Programs 

Willie E. May 

Associate Directory for Laboratory Programs 

This publication is available free of charge from 

http://dx.doi.org/10.6028/NIST.IR.7880-32 

December, 2014 

U.S. Department of Commerce 

Penny Pritzker, Secretary 

National Institute of Standards and Technology 

Willie E. May, Acting Under Secretary of Commerce for Standards and Technology and Acting Director 
(This page intentionally blank) 

ii
 
 

 

 

 

 

Abstract 

The National Institute of Standards and Technology coordinates the Micronutrients Measurement 

Quality Assurance Program (MMQAP) for laboratories that measure fat- and water-soluble vitamins 

and carotenoids in human serum and plasma. This report describes the design of and results for the 

Winter, Spring and Fall 1992 MMQAP measurement comparability improvement studies: 1) Round 

Robin XXIV Fat-Soluble Vitamins and Carotenoids in Human Serum, 2) Round Robin XXV FatSoluble Vitamins and Carotenoids in Human Serum, 3) Round Robin XXVI Fat-Soluble Vitamins 

and Carotenoids in Human Serum, and 4) Round Robin 3 Ascorbic Acid in Human Serum. The 

materials for Round Robin XXIV were shipped to participants in January 1992; participants were 

requested to provide their measurement results by March 6, 1992. The materials for Round Robin 

XXV were shipped to participants in May 1992; participants were requested to provide their 

measurement results by June 26, 1992. The materials for Round Robin XXVI were shipped to 

participants in August 1992; participants were requested to provide their measurement results by 

October 16, 1992. The sample materials for Round Robin 3 were distributed in August 1992 with 

results due by September 26, 1992. 

Keywords 

Human Serum 

Retinol, α-Tocopherol, γ-Tocopherol, Total and Trans-β-Carotene 

Ascorbic Acid 

iii 
 

 

 

 

 

 

 

 

 

 

 

 

Table of Contents 

Abstract............................................................................................................................................... iii
 

Keywords ............................................................................................................................................ iii
 

Table of Contents ............................................................................................................................... iv
 

Introduction......................................................................................................................................... 1
 

Round Robin XXIV: Fat-Soluble Vitamins and Carotenoids in Human Serum......................... 1
 

Round Robin XXV: Fat-Soluble Vitamins and Carotenoids in Human Serum .......................... 2
 

Round Robin XXVI: Fat-Soluble Vitamins and Carotenoids in Human Serum......................... 2
 

Round Robin 3: Vitamin C in Human Serum................................................................................. 3
 

References ............................................................................................................................................ 3
 

Appendix A. Shipping Package Inserts for RR24........................................................................ A1
 

Appendix B. Final Report for RR24 ..............................................................................................B1
 

Appendix C. “Individualized Report” for RR24 ..........................................................................C1
 

Appendix D. Revised “All-Lab Report” for RR24 ...................................................................... D1
 

Appendix E. Shipping Package Inserts for RR25 ......................................................................... E1
 

Appendix F. Final Report for RR25............................................................................................... F1
 

Appendix G. Revised “All-Lab Report” for RR25 ....................................................................... H1
 

Appendix H. Shipping Package Inserts for RR26.......................................................................... I1
 

Appendix I. Final Report for RR26................................................................................................. J1
 

Appendix J. Revised “All-Lab Report” for RR26 ........................................................................ L1
 

Appendix K. Shipping Package Inserts for RR03........................................................................ M1
 

Appendix L. Final Report for RR03 ............................................................................................. N1
 

Appendix M. Revised “All-Lab Report” for RR03...................................................................... O1
 

iv 
 

 

 

 

 

 

 

 

Introduction 

Beginning in 1988, the National Institute of Standards and Technology (NIST) has coordinated the 

Micronutrients Measurement Quality Assurance Program (MMQAP) for laboratories that measure 

fat- and water-soluble vitamins and carotenoids in human serum and plasma. The MMQAP 

provides participants with measurement comparability assessment through use of interlaboratory 

studies, Standard Reference Materials (SRMs) and control materials, and methods development and 

validation. Serum-based samples with assigned values for the target analytes (retinol, alphatocopherol, gamma/beta-tocopherol, trans- and total beta-carotene, and ascorbic acid) and 

performance-evaluation standards are distributed by NIST to laboratories for analysis. 

Participants use the methodology of their choice to determine analyte content in the control and 

study materials. Participants provide their data to NIST, where it is compiled and evaluated for 

trueness relative to the NIST value, within-laboratory precision, and concordance within the 

participant community. NIST provides the participants with a technical summary report concerning 

their performance for each exercise and suggestions for methods development and refinement. 

Participants who have concerns regarding their laboratory’s performance are encouraged to consult 

with the MMQAP coordinators. 

All MMQAP interlaboratory studies consist of individual units of batch-prepared samples that are 

distributed to each participant. For historical reasons these studies are referred to as “Round 

Robins”. The MMQAP program and the nature of its studies are described elsewhere. [1,2] 

Round Robin XXIV: Fat-Soluble Vitamins and Carotenoids in Human Serum 

Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin 

XXIV comparability study (hereafter referred to as RR24) received four lyophilized human serum 

test samples for analysis. Unless multiple vials were previously requested, participants received one 

vial of each serum. These sera were shipped on dry ice to participants in January 1992. The 

communication materials included in the sample shipment are described in Appendix A. 

Participants are requested to report values for all fat-soluble vitamin-related analytes that are of 

interest to their organizations. Not all participants report values for the target analytes, and some 

participants report values for non-target analytes. 

The final report delivered to every participant in RR24 is reproduced as Appendix B. This report 

included: 

• Our analysis of the participants’ results. 

• Tabular presentations of all participant results 

Each participant also received an “Individualized Report” that graphs their results for selected 

analytes. An example “Individualized Report” is reproduced as Appendix C. 

Appendix D lists all of the measurement results reported for RR24 in a more accessible format. 

1
 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Round Robin XXV: Fat-Soluble Vitamins and Carotenoids in Human Serum 

Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin 

XXV comparability study (hereafter referred to as RR25) received four lyophilized human serum 

test samples for analysis. Unless multiple vials were previously requested, participants received one 

vial of each material. These sample materials were shipped on dry ice to participants in May 1992. 

The communication materials included in the sample shipment are described in Appendix E. 

Participants are requested to report values for all fat-soluble vitamin-related analytes that are of 

interest to their organizations. Not all participants report values for the target analytes, and some 

participants report values for non-target analytes. 

The final report delivered to every participant in RR25 is reproduced as Appendix F. This report 

included: 

• Our analysis of the participants’ results. 

• Tabular presentations of all participant results 

Each participant also received an “Individualized Report” that graphs their results for selected 

analytes. This report included graphical summaries of the participant’s results relative to the 

assigned values over the previous five years and the consistency of their results for blind erplicate 

samples over the previous four years. While there is no longer an example of a RR25 Individualized 

Report, its design would have been similar to the RR24 example in Appendix C. 

Appendix G lists all of the measurement results reported for RR25 in a more accessible format. 

Round Robin XXVI: Fat-Soluble Vitamins and Carotenoids in Human Serum 

Participants in the MMQAP Fat-Soluble Vitamins and Carotenoids in Human Serum Round Robin 

XXVI comparability study (hereafter referred to as RR26) received three lyophilized and two liquidfrozen human serum test samples for analysis. Unless multiple vials were previously requested, 

participants received one vial of each material. These sample materials were shipped on dry ice to 

participants in August 1992. The communication materials included in the sample shipment are 

described in Appendix I. 

Participants are requested to report values for all fat-soluble vitamin-related analytes that are of 

interest to their organizations. Not all participants report values for the target analytes, and some 

participants report values for non-target analytes. 

It is probable that a preliminary report for RR26 was mailed to all participants shortly before the 

November 14, 1992 NIST/NCI Micronutrients Analysis Workshop, however, no version of either 

the letter or the preliminary report is available. The “Summary of 1992 Round Robin Activities” 

was mailed to every participant in the 1992 program in November 1992. This summary is 

reproduced as Appendix I. 

Each participant also received an “Individualized Report” that graphically analyzes their results for 

selected analytes. This report included graphical summaries of the participant’s results relative to 

the assigned values over the previous five years and the consistency of their results for blind 

2
 
 

 

 

 

 

 

 

replicate samples over the previous four years. While there is no longer an example of a RR26 

Individualized Report, its design would have been similar to the RR24 example in Appendix C. 

Appendix J lists all of the measurement results reported for RR26 in a more accessible format. 

Round Robin 3: Vitamin C in Human Serum 

Participants in the MMQAP Vitamin C in Human Serum Round Robin 3 comparability study 

(hereafter referred to as RR03) received two frozen serum samples of the same material. These 

samples were shipped on dry ice to participants in August 1992. The available communication 

materials included in the sample shipment are provided in Appendix K. 

The test materials were prepared by adding equal volumes of 10 % metaphosphoric acid (MPA) to 

human serum that had been spiked with ascorbic acid. Participants were asked to provide two 

results for each vial. 

No copy of a final report for RR03 as delivered to the participants is available. However, a NISTinternal Report of Analysis that presents and discusses the RR03 results was prepared. Appendix L 

presents the relevant content from this document. 

While not distributed to the participants in RR03, Appendix O presents a revised “All-Lab Report” 

that lists the results for the test materials transformed into units of μmol/mL sample. 

No “Individualized Report” was provided to the participants in RR03. 

References 

1 Duewer DL, Brown Thomas J, Kline MC, MacCrehan WA, Schaffer R, Sharpless KE, May WE, 

Crowell JA. NIST/NCI Micronutrients Measurement Quality Assurance Program: Measurement 

Repeatabilities and Reproducibilities for Fat-Soluble Vitamin-Related Compounds in Human 

Sera. Anal Chem 1997;69(7):1406-1413. 

2 Margolis SA, Duewer DL. Measurement Of Ascorbic Acid in Human Plasma and Serum: 

Stability, Intralaboratory Repeatability, and Interlaboratory Reproducibility. Clin Chem 

1996;42(8):1257-1262. 

3
 
 

 

 

Appendix A. Shipping Package Inserts for RR24 

Two items were included in each package shipped to an RR24 participant: 

•	 Cover letter. The original letter has been lost. It likely would have described the four 

sample materials (sera 160 to 163), given guidance on reconstituting these lyophilized 

samples, stated that results were due March 6, 1992 and to whom they should be sent, 

and who to contact with technical questions. 

•	 Datasheet. The following page reproduces the form. 

These items were attached to the shipping box. 

A1
 
 

 

 

 

 

 

ROUND ROBIN XXIV RESULTS FROM LABORATORY # _________ 

DATE OF ANALYSIS _____________ 

RESULTS IN ug/mL 

SAMPLE # ANALYTE RESULT 

SERUM 160 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 161 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 162 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 163 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

OPTIONAL ANALYTES : SUPPLY ONE RESULT IF AVAILABLE 

SERUM # 160 161 162 163 

TRANS-BETA-CAROTENE ______ ______ ______ ______ 

ALPHA-CAROTENE ______ ______ ______ ______ 

RETINYL PALMITATE ______ ______ ______ ______ 

GAMMA-TOCOPHEROL ______ ______ ______ ______ 

LYCOPENE (TOTAL) ______ ______ ______ ______ 

9-CIS-BETA-CAROTENE ______ ______ ______ ______ 

13-CIS-BETA-CAROTENE ______ ______ ______ ______ 

LUTEIN ______ ______ ______ ______ 

ZEAXANTHIN ______ ______ ______ ______ 

BETA-CRYPTOXANTHIN ______ ______ ______ ______ 

RECONSTITUTE SERUM SAMPLES WITH 1.0 mL OF WATER. 

NIST FAX # 301-926 8671 

RESULTS DUE BACK MARCH 6, 1992 

A2 
 

 

 

Appendix B. Final Report for RR24 

The following eight pages are the final report for RR24 as provided to all participants. 

This report consists of: 

•	 A cover letter and discussion. 

•	 Tables 1 to 3 and 7 that list the results and various summary values for total 

retinol, α-tocopherol, and total β-carotene, and γ/β-tocopherol. 

•	 Tables 4 to 6 and 8 to 13 that list the results and simple summary statistics for 

trans-β-carotene, total α-carotene, retinyl palmitate, total lutein, total lycopene, 

total zeaxanthin, total lutein & zeaxanthin, total β-cryptoxanthin, and total 

cis-β-carotene. 

Due to the complex formatting used in the Tables, the originally listed laboratory codes 

have been deleted without replacement. However, Appendix D provides a complete 

listing of the RR24 results where the original codes have been altered to ensure 

confidentiality. Appendix D also provides more relevant summary statistics. 

B1
 
B2
B3
fable 1. Round Robin lCXIV 

Ret fnot haulta ~ lia:a frcm Trillml!ld core Lib Average 

Sen.m. !el'Ull ,. ten.a .fl $erUl!I # krUlll # Ser1.1111 # Sel'Ull. tenn# Lab # 160 161 162 161 I.ab' 160 161 162 163 

o.m 

1.057 0.661 0.296 0.362 1.8 ·1.9 1.2 -5.5 0.645 0.283 0.383 ·4.1 •4.2 ·3.3 o.o 0.969 0.618 0.211 0.359 -4 .. 9 •8.3 ·6.6 ·6.2 1.oas +G.806 o.:soo +0.443 6.5 19.7 2.5 15.7 1.018 

o.m 

0.691 0.306 0.389 S.8 3.5 4.6 1.6 0.639 0.276 0.368 

o.ws ·4.5 ·5.1 ·5.,7 ·4.0 o.~ o.m 0.392 ·2.l 4.5 ·5.l 2.4 +1.140 0.690 0.310 0.410 11.9 2.5 1Z.8 7.1 +0.840 0.582 0.252 0.310 ·17.5 ·13.6 ·13.9 ·13.8 0.980 0.634 0.2$5 0.342 -3.8 ·5.9 ·12.8 ·10.7 1.07'3 0.691 O.lOZ 0.407 5.3 2.6 3.2 6.3 1.010 o.m 0.288 0.383 ·0 .. 8 •J.O -1.6 o.o 0.957 0.631 0.257 0.334 -6.0 ·6.3 -12.2 ·12.8 •1.314 0.749 0.300 0.367 J4.9 11.2 2.5 ·4.1 1.020 0.738 0.310 0.426 o.t 9.6 6.0 11.3 ~.890 0.610 0 .. 100 0.380 -12.6 •9.4 2 .. 5 -0.1 0.944 0.622 0.289 0.379 .. 7.3 -7.6 •1.2 -1.0 0.990 0.715 0.301 0.428 -2.a 6.2 2.9 11.1 1.010 0.700 o.us 0.394 5.0 l.9 o.a 2.9 0.970 0.648 0.289 0.381 -4.8 •3.8 -1.2 -o.s 1.018 0.646 0.293 0.376 -0.1 ·4.1 0.1 ·1.8 1.033 0.682 0 .. 104 0.185 1.4 1.J 3.8 0.6 1.094 0.682 0.332 0.398 7.4 1.J 13.5 4.0 1.010 0.613 0.287 0.390 -a.a ·0.1 -1.9 1.9 

o.m 

1.063 0.726 0.293 0.390 4.4 7.8 0.1 1.9 0.616 0.281 0.160 -4.0 -8.5 -4.0 ·6.0 1.0t4 0.698 0.211 l>.405 -o.s 3.6 ·1.9 5.a 1 .. ot8 0.658 0.269 0.400 -0.1 •2.3 ·8.1 4.5 +0.675 0.767 o.m 0.418 -33.7 11.9 14.3 9.2 1.040 0.715 0.2:91 +0.461 2: .. 1 6 .. 2 ·0.5 20.4 1.056 0.753 o.JQ 0.425 3.7 U.8 24.1 11.0 1.213 0.891 0 • .159 0.487 19.1 33.3 22.7 27.2 1.039 0.6'0 0.289 0.383 2.0 •3.5 ·1..2 o.o 0.851 0.531 0.234 0.216 ·16.5 ·20.1 •20.0 -27.9 1.022 o.n1 o.:sm 0.496 0.3 8.5 30.9 29.S 0.109 0.135 0.305 0.375 -89.3 9.1 4.2 ·2.1 o.m 0.640 0.211 0.368 -J.5 •5.0 ·7.4 -J.9 o.961 o.a o.m D.360 -5.7 ·5.J ·20.4 ·6.0 1.313 1.osz 0.378 0.476 21.9 56.2 211.1 24.2 1.110 1.ao 0.713 0.044 0.441 m.6 5.9 -85.0 15.2 o.aso 0.320 0.410 an.a a.2 9.4 22.a 0.763 0.590 0.287 o.m ·25.1 ·12.4 ·2.1 ~u.5 0.490 0.380 0.200 0.220 -51 .. 9 ·43.6 •31.6 ·42.5 

AW <42) 1.002 0.681 0.288 0.381 

80 0.242 0.102 0.052 0.052 CoN Llba (29;15-W) RIO 24.2 15.0 18.2 13.6 lRIM AW 1.0t9 0.673 0.293 0.383 

Core SD 0.045 0.047 0.020 0.026 Lllbl "<29;15·97) 

AW RSO 4.4 6.9 1.0 6.7 1.012 0.618 0.293 0.388 so O.U4 0.052 0 .. 020 o.tm Miil .RIO 11.2 1.1 7.0 7.9 AW 0.945 0.604 o.m 0.355 

SD 0.048 CM:l41 0.019 o.o:so (l)llew Libs C10;98•1f5) AW 1.042 0.7'35 a.a 0.409 PREVUIJS • 0 .. 435 0.146 0.102 0.069 VAWE 1.010 0.659 0.291 0.369 ftlD 41.8 19.9 35.7 16.9 

+ • V1lut rtllOVed fOf' Con I.lb Trllllled Average. <b)Kev Llba C3;116•118> 

AW o.m 0.600 0.2:69 o.~ La Late rnulta not included in the 1tati1Uea. 80 0.374 o.m 0.062 0.125 <•> • perth:ipmtt111 for the third t9. RID 45.2 37.S a.o !6.6 Cb> • pertf c:ipmting for the first tt.. 

B4
 
Table Z. Round Robin XMtV 

Alph11•Toeopberol Re8Utts I li11s frOl!l Trillln!ed Core lab Averege 

Sena# Serll!l IJ Sert.Ill I SeM.111 # ser1.1111 ii !ilerUlll ti !ileNlll' Sen111 II lab, 160 161 162 163 Lab# 160 161 162 163 

6.28 16.55 4.62 S.72 ·1.7 3.8 0.3 1.2 5.74 16.05 4.36 5.56 •10.2 0.6 •S.4 ·1.7 +5.23 14.27 3.99 4.94 •18.2 ~11>.s •13.5 ·12.7 6.80 17.20 4.60 5.99 6.4 1.9 ·0.2 5.9 +1.04 11.63 4.95 5.88 10.2 10.6 7.4 3.9 6.21 15.97 4.45 5.63 -2.a o., ·3.5 ·O.S 6.40 15.20 4.28 5.56 0.2 ·4.7 -1.1 ·1.7 6.10 16.20 4.80 5.80 -4.5 f.6 4.2 2.5 •7.33 17.95 4.78 6.51 14.7 12.6 3.7 15.0 6.45 16.15 4.52 5.52 o.9 1.3 -1.9 ·2.5 +4.61 13.W +3.U +4.40 ·26.8 ·12.4 ·29.9 ·22.2 6.70 16.17 5.13 6.16 4.1 1.4 11.3 8.9 6.27 16.30 4.76 5.81 ·1.9 2.2 3.3 2.7 +5.40 14.0l!I 4.00 4.9S ·t5.5 ·U .. 7 ·tl.2 ·12.0 +B.09 +18.56 4.52 5.15 26.6 16.4 ~z.o ·9.0 6.29 15.77 4.sa 5.34 ·1.6 ·1.1 ·0.6 ·5.6 6.21 16.24 4.83 5.56 -2.8 1.8 4.8 -1.7 6.57 16.35 +6.62 6.31 2.8 2.5 43.7 12.6 6.01 15.68 4.79 5.IU ·6.0 ·1.7 4.0 2.1 6.96 16.25 4.91 +1.07 9.2 1.9 6.6 24.9 6.to 16.10 4.50 5.60 ·4.5 1.0 •2 .• 3 -1.0 6.28 \4.74 4.36 5.70 ·1.7 -7.5 ·5.5 o.a 6.41 15.69 4.57 s.sa D.3 ·1.6 ·0.8 ·1.4 6.76 17.25 5.07 6.37 S.8 a.2 10.0 12.6 6.16 15.20 4.34 5.36 ·3.6 ·4.7 ·S.8 ·5.3 6.83 17.62 4.82 5.75 6.9 10.5 4.6 1,6 6.09 15.47 4.78 5.65 ·4.7 ·3.o l.7 ·0.2 6.21 15.54 4.48 5.48 •2.8 ·2.6 ·2.8 ·3.2 +3.13 •18.46 5.04 5.42 ·Sl.1 15.8 9.4 ·4.3 6.19 15.0l!I 4.10 5.19 ·3.1 ·5.4 ·11.0 ·8.3 6.66 17.23 4.96 5.85 4.2 8.0 7.6 3.4 4.91 11.87 3.5'7 4.74 ·23.2 ·25.6 •22.5 ·16.2 7.20 15.50 5.00 6.70 12.7 ·2.8 8.5 11!.4 6.31 15.29 4.35 5.18 ·1.3 ·4.1 ·5.6 ·8.5 7.38 20.43 5.55 6.11 15.5 28.1 20.4 18.6 7.20 18.25 5.27 6.03 12-7 14.4 14.3 6.5 6.59 14.62 4.60 5.73 3. 1 ·8.3 ·0.3 t.3 5.50 14.26 3.81 4.72 •13.9 ·10.6 *17.3 ·16.6 7.90 17.5.2 5.66 7.30 23.6 9.9 22..8 29.0 5.30 12.67 0.82 4.83 •17.1 ·2.0.6 ·17.1 •14.7 3.46 U.87 3.56 3.30 ·45.9 ·25.6 ·22.7 ·41.7 

AVG (41) 6.23 15.95 4.61 5.64 Core Libs (J0;15•97) SD 0.91 1.n 0.60 0.73 TIUN AVG 6.39 15.95 4.61 5.66 HD 15.6 10.8 13 .. 1 12.9 SD 0.33 1.04 0.31 o.39 

tort Labs <30;15•97) RSD 5.1 6.5 6.1 7.0 

AVG 6.24 16.12 4.63 5.66 IUSf 

so 0.87 1.20 0.55 0.52 AW 6.42 16.45 4.72 5.74 RID 14.0 7.4 11.9 9.Z SD 0.44 o.S9 0.39 0.6t 

(1)New labs C8;9S•113) PR.EVIM AVG 6.47 15.93 4.66 5.71 VAUJE 6.28 16.59 4.62 S.64 SD o.er 2.64 D.69 0 .. 78 

RID 13.5 16.6 15.,0 13.7 + "' Value rltl'llMld for tort Lab Trinad Average. 

ib)New Labs <3:116-118) L"' Late reaults not Included in the atatiattcs. AW s.ss 14.02 4.35 S.14 (a) • partictpatfna fer th• thlrd time. SD 2.23 S.06 1.14 2.02 Cb> • participating for the ftrat ti•. RID 40.2 21.8 26 .. 3 39.3 

B5
 
Tabl111 3. Round Robin XXJ\I 

Total S.te•Carctene Results X Sin fn:!lll trlll'mld tore Lab Average 

S&rLlll # Sann # S11r1.111 # Sctrl..lll # StiN.111 # sert.m # StirUll # serun # Lab # 160 l61 162 163 Lab # 160 161 162 t63 

0.1394 2.539 t.193 0.203 3.9 14.8 11.2 4.2 0.078 2.180 0.988 0.178 ·13.7 •1.5 ·7.9 ·8.7 +0.043 1.979 1.074 0.181 ·53.0 ·10.5 0.1 ·7.1 0.092 2.294 1.001 0.182 1.7 3.7 ·6.7 ·6.6. 0.111 2.414 1.089 0.211 22.2 9.1 1.5 a.o +0.130 2.341 1.203 0.199 41.8 5.S 12.1 2.1 0.086 +3.900 +1.760 0.255 ·4.9 16.3 64.1 30.9 0.096 +2.750 1.212 0.173 6.2 24.3 13.0 ·11.2 0.092 2.300 U>JO 0.190 1.7 4.0 ·4.0 ~2.5 o.oao 2.457 1.069 0.190 ·11.5 11., ·O.l ·2.5 +0.052 1.856 +0.779 0.183 ·42.5 ·16.1 ·21.4 •6., 0.084 2.300 1.026 0.183 ·7.1 4.0 •4.4 •6.1 0.084 1.910 0.959 o.m ·7.1 •13.7 ·10.6 14.4 0.019 2.160 +0.851 0.153 .. 12.6 •2.4 ·20.7 ·21.5 0.109 2.293 1.153 0.225 20.5 3.7 7.5 15.5 0.091 +1.540 1.060 0.241 0.6 ·30.4 •1.2 23.7 o.oss 2.211 1.035 0.189 ·2.1 2.7 ·3.5 ·l.o o .. osa 1.953 o.m 0.156 "11.7 ·11.7 -12 .. 4 •19.,7 0.104 2.146 1.165 0.201 15.0 ·3.0 8.6 3.1 0.095 2.010 0.895 0.182 5.1 ·6.4 •16.6 ·6.6 +o.305 +2.873 +1.301 0.186 237.3 29.9 21.3 ·4 .. 5 0.090 +o.m 1.040 0.190 •0.5 ·19.4 ·J.1 ·2.5 0.081 1.949 0.762 0 .. 132 ·10.4 ·11.9 ·29.0 ·32.3 0.166 1.raa 0.958 0.173 83.6 ·19.2 ·10.7 ·1t.2 0.141 2.364 1.083 0.229 55.9 6.9 1.0 17.5 0.034 0.&90 0.45D 0.069 ·62.4 ·59.8 ·58.1 ·64.6 0.114 1.965 0.921 0.184 26.1 ·11.2 ·14.1 •5.6 0.106 2.234 0.939 0.178 11.2 1.0 -12.s ~a.1 0.038 1.682 0.651 0.104 ·51.0 .. 24.0 ·39.3 ·46.6 0.154 4.635 1.137 0.126 69.9 109.S 5.9 •35.4 0.221 2.600 1.140 0.244 144.4 17.5 6.3 25.2 0.073 2.180 0.710 0.150 ·19.3 ·1.S •D.8 ·23.0 0.066 1.630 0.715 0.132 ·21.0 ·26.3 •!J .• 3 ·32.3 

AVG (33) 0.100 2.205 1.016 0.183 Core Laba C21r15·97> ID 0.051 o.ns 0.224 0.039 TRJM AVG 0.090 2.212 1.073 0.195 RSD 51.2 32.9 22 .. 0 21.5 SD 0.010 0.201 0.085 0.025 

Core Laba (21;15·97> 

RSO 11.0 9.1 7.9 12 .. 9 

AVG D.098 2.2~ 1.092 0.195 NIST lb o.ost 0.653 0.196 0.025 AVG 0.078 2.179 1.049 0.'91 ISD 51.6 29.4 17.9 12.9 ID 0.013 o.m 0.062 0.013 

(l)New L.tll C9;98•1\5) PRlVJOUS AVG 0.1t7 2.234 0.893 0.160 VALUE 0.090 2.338 1.145 0.202 SD 0.061 1.024 o.m 0.057 

ISD 52.0 45.8 26.1 35.I + • V•lue MllllO'led for tore Lib Trfmed AvenQe. 

Cb)llew Llba (2;116·117) L• Late re1Ult1 not included in the atattatica. AVG 0 .. 070 1.905 0.713 0.141 <•> • partic:tpatint fOr the thttd ti•. ID o.oos O.J89 0.004 0.013 Cb) • partlc:tpatino for the first tt•. ISO 1.1 20.4 0.5 9.0 

B6
 
Table 4. Round Robin XXIV Table s. Round Robin )()UV Tr-·&etlll*Carctene Results Alpf111-C!arotene 

Serun # 14111'1.111 # Sert.11t# S11rU11 # sorta# Sermt # S1rtn ti Serun # Lab # 160 161 162 163 Lab # 160 161 162 163 

0.083 2.352 1.089 0.185 0.026 0.101 0.038 0.012 0.086 2.140 0.980 0.180 1).(117 0.088 o.on 0.010 0.QBO 2.276 1,009 o.1ao 0.011 0.021 0.043 1.554 0.672 0.139 0.049 o.zao 0.077 o .. oeo 2.093 .0.975 0.179 0.003 0.042 O.CJ12 0.073 1.690 0.670 o. t20 0.026 0.100 0.036 0.()09 0.030 0.727 0.399 0.062 0.016 0.096 0.032 0.010 0.075 1.798 0.1111 0.163 0.020 0.074 0.029 0.013 0.113 3.883 0.941 0.126 O.Ot3 0.063 0.032 0.014 IUSf 0.072 1.900 0.947 0.181 0.015 0.086 0.018 0.005 

o.oa 0.074 0.03i 0.012 

0.014 0.121 0.054 0.()10 AVG 0.073 2.041 0.867 0.151 0.196 0.091 0.034 0.009 SD 0.023 0.1'R 0.215 0.040 0.025 0.084 0.030 o.oto RSD 31.2 39.1 24.8 26.l 0.033 0.121 0.046 D.038 o.oz1 o.093 0.028 0.009 

0.039 0.086 0.029 0.053 

0.038 0.011 0.005 Table '~ Round Robin XXtV 0.016 0.079 0.037 0.019 htinyt Palmitate 0.229 0.046 

NIST 0.018 o.091 0.034 0.010 

S11N11 # lenn # Ser1.111 # 8erun # 

lab # 160 161 16Z 163 AVG 0.031 0.103 0.034 0.015 

SD 0.041 Cl.056 0.014 0.012 0.010 0.024 RSO 133.6 54.7 41.0 84.4 0.020 0.035 o.ooa 0.031 

0.1&1 0.081 0.026 0.030 

0.040 0.026 

0.115 0.080 0.041 0.064 

AVG 0.062 0.052 0.025 0.038 

so 0,0.54 0.027 0.017 0.018 

llSO 88.0 51.2 67.0 46.5 

Table 7. Round Robin IOUV X liliH fran Trtmed Lib Average G#llltll·Tccopberol 

Serun # Sena• Stf'Ulll ti kn.a' senn • le1111 II SertA ti Serun # lab# 160 t61 162 163 lab# 160 161 162 163 

1.70 4.09 1.64 3.59 4.8 12.9 0.1 6.5 1.60 3.80 1.60 3.40 ·1.4 4.9 ·2.2 0.8 1.30 3.60 1.60 3.20 ·19.9 •0.6 •2.2 ·5.1 1.57 3.61 t.56 3.24 •3.3 ·0.4 ·4.7 ·3.9 1.96 3.85 1.95 3.71 20.8 6.3 19.Z 10.0 1.61 3.64 1.64 J.28 2.9 0.5 0.2 ·2.7 1.45 3.45 t.51 3.07 ·t0.6 ·4.8 ·7.7 •8.9 *2.36 *4.47 t.82 3.41 60.2 23.4 u.2 1.1 1.75 3.73 2.04 3.24 7.8 2.9 24.7 ·3.9 1.ea 3.75 1.77 3.67 15.8 J.4 8.2 8.9 1.78 3.68 1.13 3.45 9.7 1.6 5.7 2.3 1.77 3.28 1.44 3.61 9.1 ·9.5 •12.0 13.0 •o.s1 111 1.18 1110.54 *1.04 ·67.3 •67.4 •67.0 ·69.2 1.40 3.38 t.45 3.10 ·13.8 ·6.8 ·11.7 ·7.9 1.38 l.44 1.26 3.07 ·14.9 ·5.1 ·21.7 ·8.9 *1.(14 *2.91 *1.08 *2.27 ·35.9 •19.7 ·34.0 •32.7 Hf ST 1.51 l.43 1.52 3.32 

AVG 1.57 3.49 1.54 3.17 

• • Value ~ for the TllMNED avoraee. 

ID 0.40 0.69 0.35 0.65 

RSD 25.4 19.6 22.5 20.5 

l'IHIMED 

AVG 1.62 3.62 t.64 3.31 

ID 0.20 0.22 0.20 0.24 

RID 12.2 6.0 t2 .. 2 7.0 

B7
 
fable 8. AOU1d Robin UlV table 9. ROI.rid Robin XMIV I.Uta in L~ 

lorun # Serun # Serua # Scrua # SONI!# Sl!f'l.D # SGl"U'lll # S1trun # Lab# 160 161 162 163 Lab # 160 161 162 163 

0.067 0.086 0.053 0.045 0.824 0.339 0.205 0.168 0.055 0.079 0.045 0.039 0.754 0.347 0.200 0.166 0.109 0.138 C.081 0.068 l'l.845 0.312 0 .. 198 0.142 0.073 0.093 0.047 0.049 1.066 0.362 0.219 0.168 0.174 0.196 O.t01 0.152 1.175 0.563 0.344 0.265 0.062 0.08\ 0.048 0.045 0.484 0.210 0.120 0.102 0.091 0.147 0.082 0.093 o.m 0.351 0.181 0.16\ 0.045 l).043 0.026 0.027 0.183 0.146 0.064 0.068 0.030 0.045 0.029 0.020 1.235 0.416 0.195 0.204 

NIST 

0.182 0.114 0.310 o.m 0.290 0.143 0.121 0.012 0.079 0.049 0.021 D.4t6 0.175 o.tn 0.091 

AVG 0.910 0.486 0.341 o.m 0.078 0.106 0.062 o.oao 0.747 o.m 0.165 0.128 so 0.040 0.052 0.030 0.085 0.642 0.217 o.1oz 0.114 1110 51.9 48.8 48.0 101.1 0.806 0.484 0.237 0.167 

0.646 D.218 0.122 0.100 

0.621 0.281 0.134 0.121 

0 .. 115 0.106 0.011 0.052 

0.638 o.m 0.136 0.125 

0.112 0.114 0.310 

NIST o.m 0.316 0.182 0.139 

AW 0 .. 730 0.305 0.111 0.\53 so 0.261 0.118 0.074 0.068 RIO 35.8 38.8 43.3 44.4 

tabt1t 10. Round lobin lCXIV Teble 11. Round Robin UlV Zeaxanthin 1.utetn + Zeax!S\tbin 

terca # aer1111 • leNll. Serllll # Sena# Senn. lelUl'I. Senn # Lab I 160 161 162 t63 Lebl 160 16' 162 163 

0.010 0.022 0.013 0.012 D.088 0.110 0.014 0.065 D.019 0.021 O.Ot9 0.021 0.121 0.166 0.098 o.oas 0.015 0.021 0.015 0.015 0.095 o.t:si 0.077 0.067 0.011 o.oz1 0.015 0.011 0.057 0 .. 076 0.050 o.oso 0.010 0.040 0.091 

JUST 0.038 0.036 G.026 0.025 AW 0.090 0.121 0.075 G.067 ID D.029 0.038 0.020 G.014 AW 0.019 o.m 0.021 0.029 ISO 32.7 31.3 26.3 21.s ID o.on 0.019 0.010 0.031 !lSD 61.4 58.2 48.0 105.5 

B8
 
Table 12. ROLl'ld Robin XXtV Tele t3.IOU"ld Robin XXIV 

S.ta•CryptOKSlthin 9+1S Cis·letrCarotcM 

Serl.P # Sltl'l.lll # leri,a # Serwt I llMat 1«1.111 # Str1.111 # s~run f 

Lab f 160 161 162 163 Lab# 160 161 162 163 

0.057 0.061 o.~ 0.034 0.008 0.163 0.051 0.014 

0.046 0.063 0.042 0.031 

0.124 o .. n1 0.0$6 0.038 

O.CQ 0.06$ 0.841 0.035 

0.031 o.m 0.022 0.021 

0.065 0.066 CUJ31 0.031 

0.165 0.086 0.1.161 0.063 

o.oas 0.110 0.066 0.052 

0.037 0.058 o.mo 0.026 

0.094 0.062 0.035 0.014 

0.1'7 0 .. 090 0.068 0.060 

0.239 0.155 0.103 0.065 

0.031 0.021 0.018 0.015 

0.037 o.m 0 .. 041 0.037 

fUIT 0.038 IJ.0!7 0.025 0.020 

AW 0.082 o.on 0.046 0.037 

IO 0.059 0.014 0.023 0.016 

HD 11.9 47.0 49.5 42.0 

B9
 
 

 

Appendix C. Representative “Individualized Report” for RR24 

Each participant in RR24 received graphical summaries of their own measurement 

performance for total retinol, α-tocopherol, and/or total β-carotene. In RR24, two sets of 

graphs were prepared: 

•	 “Percent Bias” relative to the “Trimmed Core Lab Average” for of the serumbased samples distributed from 7/1987 through 1/92. 

•	 “Blind Duplicate Performance”, documenting the history of the % Bias values for 

just the sera distributed in RR24. 

The following six pages constitute the individualized report for participant FSV-BA. 

C1
 
Laboratory FSV-BA 

% Bias 

Blind Duplicate Performance 

Retinal 

20 I · · · · · · · · · · · .;·. · · · · · · · · · · · · · · · · · · · · · · · · " ·· · · · · · · · · · · · · · · · · · · · ·· · · · · · · · · · · · 

1 0 I . . . . . . . . . . . • .. . · •• • . . . . . . . . . • . . . . . . . . . . . • • . . . •. ' . . . • . . . . . . . . . . • . . . . . . . . . . 

No 0 . c. ··. 

data 

-10 •··· · ········ ·· · ··-············· · ·················· · ············ ······· 

-20 •·· · ··········· · · · ····· ················ · ·· ······ ·· ············· ·· ······· 

Serum # 157 160 150 161 132 162 78 163 

8/91 1/92 5/91 1/92 5/90 1/92 1/88 1/92 

C2
 
% Bias 

Laboratory FSV-BA 

Blind Duplicate Performance 

Alpha-Tocopherol 

20 I · · · · · · ··· · · · · · .. ;•: ·:·. ··:·:· . . . ' . ·:\ .. ·; ' ·. :\ . . . , ·:", ·:·':: .. . ''.'.:'· .. . , d ' :;:•::: . . . . ; . . 

• 

·;t::(- ..... r .. , ..::-jj:: : H:'l 

.. 

1 0 I .. .. • .•.. • • ...... ... .....•. ..•.. , .. • ... • ....•. • • • • .. . · . ... • .. . . .. . . 

•••. . • . I I '" No I I I I r 11 0 I ' ' I I · I I data " · 

... 

-1 0 I . . . . . . . . . . . . . . . . . • . ' . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . · .. ' 

.. 

··: . ..:: ··: .:·- .. r·"_. :: 

-20 . · ., ;·. .:· ·· ···· ············ ·· · ····· ·····•• .1' ••·"·.·· ····· ··: · ... ........... . 

Serum # 157 160 150 161 132 162 78 163 

8/91 1/92 5/91 1/92 5/90 1/92 1/88 1/92 

C3
 
% Bias 

Laboratory FSV-BA 

Blind Duplicate Performance 

Total Beta-Carotene 

30 I "'''·"'· ·:.·.:",c. '··'···· .. · · ····· · .... ···· .. ... .. ... · · ... · ..... ···· · .... , ..... , ......... I 

20 

... 

:1· !:i';: ;::::;· ... " :Ll : i i: i:; ... ·:: 

10 1 ··· ·· · · ····· · " ···-··· · · · • .. • • • • .. .. -+ • .. • .. .. .. .. • .. ;.. .. . • .. .. • .. _ .. .. • • 

!:iji 

'":!;: 

0 I !·.W§ ""' . . ,. . I : " . '·'· . I No 

data 

-10 

.... :. . .::;: :: ...... :i., .:· ::; ..... 

.. .... .. .. ..... .. ........ ....... ... . .. .. . .. . . ... .. 

··- ::-- ·· ................ .... . -.····:······- "':,· ·;6 

•:· 

-20 ..... .. . ... ,. ••• , • • • •• •• ••• • ••• • • • • • J .. .. .. ...... . ..... . .. ... . .. ..... .. . .. - ·· 

··:· 

Serum # 157 160 150 161 132 162 78 163 

8/91 1/92 5/91 1/92 5/90 1/92 1/88 1/92 

C4
 
Percent Bias 

Laboratory FSV-BA 

Retlnol 

20 I-.... .. •. .........• . ... .•. . ... .. .... .. .... . ... .... . ... ..•...••.•.•... 

1 0 I-.. .•.. ...•...••......... ... . .. .. ...• .. ... . .••.••.••••...•..•....•.. • 

0 

-10 --- .. - - . - - -- .... . -·--. -.... -.• - - ... - - -.. --..... -. .. -.. - - . -- . - -- - ... - . 

-20 .. -. - - ... -- -..... - .. 

--

..... 

-

.... 

-

.... 

-

............. 

-

. 

-

......... 

- -

·• ... .. 

-

. 

-30 7/ 87 1/88 7/88 9/llll 1/ 89 4/ 119 8/ 119 1/90 5/ 90 9/90 1/ 91 5/ 91 8 /91 1/92 

% Bias from Assigned Values 

C5
 
Percent Blas 

Laboratory FSV-BA 

Alpha-Tocopherol 

20 ·········-········· ··-··-···- · · ············· ·· ············ 

10 .............. . .... .. .. . .. ... ........... . ............. 

0 1 ••••• i 

-10 

-20 . -. .. .. ......... 

-

..... 

-

. 

-

... . .... 

-

.............................. 

-

.... . 

-30 7/87 1/88 7/88 t /H t /et 4/88 8/et t / 80 5/tO t /tO ''" 5/tt ' ' " t / t2 

% Blas from Assigned Values 

C6
 
Percent Bias 

Laboratory FSV-BA 

Total Beta-Carotene 

20 

10 

0 

-10 ............ .................... '.;'"""" . ....................... . 

-20 

-30 7/ 87 1 /88 7 /88 9/88 1 / 811 4/89 8/89 1 /90 5 /9 0 9/ 9 0 1/ 91 5/ 91 8 /91 1/92 

% Bias from Assigned Values 

C7
 
 

 

 

 

 

Appendix D. Updated “All-Lab Report” for RR24 

The following six pages are a modernized version of an “All-Lab” report for RR24. This 

report has three parts: 

•	 pages 1 thru 4 list results for all analytes reported by at least twice, counting both 

participants and NIST analysts. 

•	 page 5 provides a legend for pages 1 thru 4. 

•	 page 6 summarizes each participants’ performance for total retinol, α- and γ/βtocopherol, and total β-carotene. These summaries are compatible with the 

percent bias evaluation advice given in the RR24 Report. However, the current 

bias summaries are estimated relative to the median of all reported values for each 

analyte in each serum rather than to the “Trimmed Core Lab Average” used in the 

original and detailed in Appendix B. These original reference values were 

estimated from on-time results of the more experienced participants, with 

subjective exclusion of results deemed non-representative. 

To ensure confidentiality, the laboratory identifiers used in this “All-Lab Report” have 

been altered from those used in RR24. The only attributed results are those reported by 

NIST. The NIST results are not used in the assessment of the consensus summary results 

of the study. 

Note: The “NIST” values in the Tables described in Appendix B are the average of the 

NISTa, NISTb, and NISTc results. 

D1
 
 

Round Robin XXIV Laboratory Results 

Total Retinol, μg/mL Retinyl Palmitate, μg/mL α-Tocopherol, μg/mL γ/β-Tocopherol, μg/mL 

Lab 160 161 162 163 

FSV-BA 1.01 0.653 0.288 0.383 

FSV-BD 1.00 0.704 0.277 0.392 

FSV-BE 0.98 0.634 0.255 0.342 

FSV-BF 1.14 0.690 0.330 0.410 

FSV-BG 0.97 0.618 0.273 0.359 

FSV-BH 0.96 0.631 0.257 0.334 

FSV-BI 0.98 0.645 0.283 0.383 

FSV-BJ 1.02 0.646 0.293 0.376 

FSV-BK 1.03 0.682 0.304 0.385 

FSV-BL 0.99 0.715 0.301 0.428 

FSV-BM 0.97 0.648 0.289 0.381 

FSV-BN 1.09 0.735 0.305 0.375 

FSV-BO 1.23 0.830 0.320 0.470 

FSV-BP 1.02 0.731 0.383 0.496 

FSV-BS 1.31 1.052 0.378 0.476 

FSV-BX 

FSV-BY 1.06 0.661 0.296 0.362 

FSV-CA 1.08 0.697 0.306 0.389 

FSV-CB 0.85 0.538 0.234 0.276 

FSV-CH !3.25 0.767 0.335 0.418 

FSV-CJ 1.09 0.806 0.300 0.443 

FSV-CK 1.37 0.749 0.300 0.367 

FSV-CL 1.06 0.753 0.363 0.425 

FSV-CM 

FSV-CO 0.97 0.639 0.276 0.368 

FSV-CP 

FSV-CQ 0.84 0.582 0.252 0.330 

FSV-CS 1.07 0.700 0.295 0.394 

FSV-CT 1.87 0.713 0.044 0.441 

FSV-CU 0.98 0.616 0.281 0.360 

FSV-CV 1.01 0.673 0.287 0.390 

FSV-CY 1.02 0.738 0.310 0.426 

FSV-DC 1.07 0.691 0.302 0.407 

FSV-DE 

FSV-DL 1.02 0.658 0.269 0.400 

FSV-DM 1.21 0.898 0.359 0.487 

FSV-DS 0.76 0.590 0.287 0.335 

FSV-DW 

FSV-DY 0.94 0.622 0.289 0.379 

FSV-EA 1.04 0.650 0.289 0.383 

FSV-EB 1.01 0.698 0.287 0.405 

FSV-EC 1.04 0.646 0.286 0.395 

FSV-EF 0.89 0.610 0.300 0.380 

FSV-EI 0.96 0.638 0.233 0.360 

FSV-EJ 1.04 0.715 0.291 0.461 

FSV-EN 0.49 0.380 0.200 0.220 

FSV-EV 1.06 0.726 0.293 0.390 

FSV-EY 1.09 0.682 0.332 0.398 

FSV-FM 0.98 0.640 0.271 0.368 

160 161 162 163 

0.101 0.081 0.026 0.030 

0.020 0.035 0.008 0.031 

nd 0.040 nd 0.026 

nd nd nd nd 

nd nd nd nd 

0.010 0.024 nd nd 

0.115 0.080 0.041 0.064 

160 161 162 163 

6.27 16.3 4.76 5.81 

6.40 15.2 4.28 5.56 

4.68 14.0 3.23 4.40 

6.10 16.2 4.80 5.80 

5.23 14.3 3.99 4.94 

5.40 14.1 4.00 4.98 

5.74 16.1 4.36 5.56 

6.28 14.7 4.36 5.70 

6.41 15.7 4.57 5.58 

6.98 16.3 4.91 7.07 

6.10 16.1 4.50 5.60 

7.20 18.2 5.27 6.03 

7.90 17.5 5.66 7.30 

7.38 20.4 5.55 6.71 

6.28 16.5 4.62 5.72 

7.04 17.6 4.95 5.88 

6.31 15.3 4.35 5.18 

!0.70 18.5 5.04 5.42 

6.80 17.2 4.60 5.99 

8.09 18.6 4.52 5.15 

6.66 17.2 4.96 5.85 

6.01 15.7 4.79 5.81 

6.21 16.0 4.45 5.63 

7.33 18.0 4.78 6.51 

6.09 15.5 4.78 5.65 

6.16 15.2 4.34 5.36 

6.29 15.8 4.58 5.34 

6.70 16.2 5.13 6.16 

6.45 16.2 4.52 5.52 

4.91 11.9 3.57 4.74 

5.30 12.7 3.82 4.83 

6.57 16.4 6.62 6.37 

7.20 15.5 5.00 6.70 

6.21 15.5 4.48 5.48 

6.80 15.9 5.15 6.57 

6.21 16.2 4.83 5.56 

5.50 14.3 3.81 4.72 

6.19 15.1 4.10 5.19 

3.46 11.9 3.56 3.30 

6.83 17.6 4.82 5.75 

6.76 17.3 5.07 6.37 

6.59 14.6 4.60 5.73 

160 161 162 163 

1.67 3.64 1.64 3.28 

1.30 3.60 1.60 3.20 

1.45 3.45 1.51 3.07 

1.60 3.80 1.60 3.40 

1.88 3.75 1.77 3.67 

1.40 3.38 1.45 3.10 

1.70 4.09 1.64 3.59 

2.36 4.47 1.82 3.41 

0.53 1.18 0.54 1.04 

1.78 3.68 1.73 3.45 

1.96 3.85 1.95 3.71 

1.57 3.61 1.56 3.24 

1.75 3.73 2.04 3.24 

1.38 3.44 1.28 3.07 

1.77 3.28 1.44 3.81 

1.04 2.91 1.08 2.27 

n 43 44 44 44 

Min 0.490 0.380 0.044 0.220 

Mean 1.037 0.684 0.289 0.390 

Max 1.870 1.052 0.383 0.496 

SD 0.189 0.099 0.052 0.051 

CV 10 9 13 10 

4 5 3 4 

0.010 0.024 0.008 0.026 

0.062 0.052 0.025 0.038 

0.115 0.081 0.041 0.064 

0.054 0.027 0.017 0.018 

47 33 41 27 

41 

3.46 

6.32 

8.09 

0.85 

11 

42 42 42 

11.9 3.23 3.30 

15.9 4.62 5.66 

20.4 6.62 7.30 

1.7 0.60 0.73 

8 9 10 

16 16 16 16 

0.53 1.18 0.54 1.04 

1.57 3.49 1.54 3.16 

2.36 4.47 2.04 3.81 

0.41 0.71 0.36 0.67 

17 16 17 18 

NISTa 0.905 0.599 0.279 0.336 

NISTb 0.932 0.565 0.252 0.339 

NISTc 0.998 0.647 0.288 0.389 

5.92 

6.58 

6.76 

15.9 4.28 5.13 

17.1 5.01 6.35 

16.4 4.87 5.75 

1.60 3.65 1.55 3.43 

1.61 3.60 1.65 3.40 

1.32 3.05 1.36 3.14 

Median 1.018 0.678 0.290 0.387 

eSD 0.071 0.058 0.020 0.032 

eCV 7 9 7 8 

0.040 

0.024 

59 

6.29 16.01 4.60 5.64 

0.61 1.29 0.42 0.48 

10 8 9 9 

1.64 3.63 1.60 3.26 

0.31 0.27 0.23 0.28 

19 7 15 9 

D2
 

Revised "All Lab Report" Page 1 / 6 
Round Robin XXIV Laboratory Results 

Total β-Carotene, μg/mL trans-β-Carotene, μg/mL Total cis-β-Carotene, μg/mL 

Lab 160 161 162 163 

FSV-BA 0.092 2.30 1.03 0.190 

FSV-BD 

FSV-BE 

FSV-BF 0.130 2.34 1.20 0.199 

FSV-BG 0.043 1.98 1.07 0.181 

FSV-BH 0.080 2.46 1.07 0.190 

FSV-BI 0.078 2.18 0.99 0.178 

FSV-BJ 0.109 2.29 1.15 0.225 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.114 1.97 0.99 0.184 

FSV-BO 0.073 2.18 0.71 0.150 

FSV-BP 0.141 2.36 1.08 0.229 

FSV-BS 0.154 4.64 1.14 0.126 

FSV-BX 0.084 2.30 1.03 0.183 

FSV-BY 0.094 2.54 1.19 0.203 

FSV-CA 

FSV-CB 

FSV-CH !0.31 2.87 1.30 0.186 

FSV-CJ 0.092 2.29 1.00 0.182 

FSV-CK 0.052 1.86 0.78 0.183 

FSV-CL 0.081 1.95 0.76 0.132 

FSV-CM 

FSV-CO 0.111 2.41 1.09 0.211 

FSV-CP 0.080 1.95 0.94 0.156 

FSV-CQ 0.086 3.90 1.76 0.255 

FSV-CS 

FSV-CT 0.221 2.60 1.14 0.244 

FSV-CU 0.088 2.27 1.04 0.189 

FSV-CV 0.091 1.54 1.06 0.241 

FSV-CY 0.084 1.91 0.96 0.223 

FSV-DC 0.096 2.75 1.21 0.173 

FSV-DE 

FSV-DL 0.095 2.07 0.90 0.182 

FSV-DM 0.166 1.79 0.96 0.173 

FSV-DS 0.066 1.63 0.72 0.132 

FSV-DW 0.034 0.89 0.45 0.069 

FSV-DY 0.079 2.16 0.85 0.153 

FSV-EA 

FSV-EB 0.104 2.15 1.17 0.201 

FSV-EC 0.112 1.65 1.26 0.217 

FSV-EF 

FSV-EI 0.038 1.68 0.65 0.104 

FSV-EJ 0.090 0.24 1.04 0.190 

FSV-EN 

FSV-EV 

FSV-EY 

FSV-FM 0.106 2.23 0.94 0.178 

160 161 162 163 

0.086 2.14 0.98 0.180 

0.080 2.28 1.01 0.180 

0.075 1.80 0.92 0.163 

0.113 3.88 0.94 0.126 

0.083 2.35 1.09 0.185 

0.043 1.55 0.67 0.139 

0.073 1.69 0.67 0.120 

0.080 2.09 0.98 0.179 

0.030 0.73 0.40 0.062 

160 161 162 163 

0.006 0.16 0.05 0.010 

0.000 0.18 0.06 0.010 

0.039 0.17 0.07 0.021 

0.042 0.75 0.20 nd 

0.011 0.19 0.10 0.018 

0.009 0.30 0.11 0.044 

0.008 0.26 0.09 0.012 

0.008 0.18 0.06 0.010 

0.004 0.16 0.05 0.007 

n 33 34 34 34 9 9 9 9 9 9 9 8 

Min 0.034 0.24 0.45 0.069 0.030 0.73 0.40 0.062 0.000 0.16 0.05 0.007 

Mean 0.096 2.19 1.02 0.183 0.074 2.06 0.85 0.148 0.014 0.26 0.09 0.017 

Max 0.221 4.64 1.76 0.255 0.113 3.88 1.09 0.185 0.042 0.75 0.20 0.044 

SD 0.037 0.73 0.23 0.039 0.024 0.84 0.22 0.041 0.015 0.19 0.05 0.012 

CV 17 16 13 15 22 22 20 22 37 25 24 27 

NISTa 0.090 2.40 1.12 0.204 

NISTb 0.065 1.96 1.02 0.190 0.063 1.62 0.86 0.189 0.002 0.34 0.15 0.001 

NISTc 0.080 2.18 1.01 0.179 0.081 2.18 1.03 0.172 nd nd nd 0.007 

Median 0.091 2.180 1.033 0.184 0.080 2.093 0.941 0.163 0.008 0.181 0.066 0.011 

eSD 0.019 0.345 0.157 0.027 0.009 0.437 0.101 0.033 0.004 0.027 0.024 0.004 

eCV 21 16 15 15 11 21 11 20 56 15 36 34 

D3

Revised "All Lab Report" Page 2 / 6 
 

Round Robin XXIV Laboratory Results 

Total α-Carotene, μg/mL Total Lycopene, μg/mL Total β-Cryptoxanthin, μg/mL 

Lab 160 161 162 163 

FSV-BA 0.026 0.100 0.036 0.009 

FSV-BD 

FSV-BE 

FSV-BF 0.049 0.280 0.077 nd 

FSV-BG 

FSV-BH 0.016 0.096 0.032 0.010 

FSV-BI 0.017 0.088 0.032 0.010 

FSV-BJ 0.023 0.074 0.031 0.012 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.016 0.079 0.037 0.019 

FSV-BO 

FSV-BP 0.039 0.086 0.029 0.053 

FSV-BS nd 0.229 0.046 nd 

FSV-BX 0.013 0.083 0.032 0.014 

FSV-BY 0.026 0.101 0.038 0.012 

FSV-CA 

FSV-CB 

FSV-CH 

FSV-CJ 0.017 nd 0.021 nd 

FSV-CK 0.020 0.074 0.029 0.013 

FSV-CL 0.021 0.093 0.028 0.009 

FSV-CM 

FSV-CO 

FSV-CP 0.196 0.091 0.034 0.009 

FSV-CQ 

FSV-CS 

FSV-CT 

FSV-CU 

FSV-CV 0.014 0.121 0.054 0.010 

FSV-CY 

FSV-DC 0.003 0.042 0.012 nd 

FSV-DE 

FSV-DL 0.025 0.084 0.030 0.010 

FSV-DM 

FSV-DS 

FSV-DW 0.038 0.017 0.005 

FSV-DY 0.015 0.086 0.018 <0.005 

FSV-EA 

FSV-EB 

FSV-EC 

FSV-EF 

FSV-EI 

FSV-EJ 0.033 0.121 0.046 0.038 

FSV-EN 

FSV-EV 

FSV-EY 

FSV-FM 

160 161 162 163 

0.48 0.21 0.120 0.102 

0.79 0.35 0.181 0.161 

0.75 0.35 0.200 0.166 

0.42 0.18 0.111 0.091 

0.64 0.27 0.136 0.125 

0.62 0.28 0.134 0.121 

1.24 0.42 0.195 0.204 

0.82 0.34 0.205 0.168 

1.07 0.36 0.219 0.168 

0.85 0.37 0.198 0.142 

0.18 0.15 0.064 0.068 

0.65 0.22 0.122 0.100 

0.75 0.28 0.165 0.128 

0.91 0.49 0.341 0.293 

1.18 0.56 0.344 0.265 

0.64 0.22 0.102 0.114 

0.32 0.11 0.077 0.052 

0.73 0.29 0.143 0.127 

0.81 0.48 0.237 0.167 

160 161 162 163 

0.062 0.065 0.041 0.035 

0.031 0.035 0.022 0.021 

0.046 0.063 0.042 0.031 

0.037 0.053 0.041 0.037 

0.239 0.155 0.103 0.065 

0.165 0.086 0.067 0.063 

0.057 0.061 0.042 0.034 

0.124 0.111 0.056 0.038 

0.065 0.066 0.031 0.031 

0.117 0.090 0.068 0.060 

0.037 0.058 0.030 0.026 

0.094 0.062 0.035 0.034 

0.031 0.027 0.018 0.015 

0.085 0.110 0.066 0.052 

n 18 19 20 15 19 19 19 19 14 14 14 14 

Min 0.003 0.038 0.012 0.005 0.18 0.11 0.064 0.052 0.031 0.027 0.018 0.015 

Mean 0.032 0.103 0.034 0.016 0.73 0.31 0.173 0.145 0.085 0.074 0.047 0.039 

Max 0.196 0.280 0.077 0.053 1.24 0.56 0.344 0.293 0.239 0.155 0.103 0.065 

SD 0.042 0.058 0.014 0.013 0.27 0.12 0.077 0.061 0.060 0.034 0.023 0.015 

CV 22 21 19 24 22 22 22 21 25 22 22 24 

NISTa 

NISTb 0.019 0.106 0.035 0.012 0.88 0.31 0.178 0.162 0.043 0.038 0.024 0.020 

NISTc 0.017 0.076 0.034 0.009 0.68 0.32 0.185 0.116 0.033 0.037 0.026 0.019 

Median 0.021 0.088 0.032 0.010 0.747 0.290 0.165 0.128 0.064 0.064 0.042 0.035 

eSD 0.008 0.018 0.007 0.003 0.162 0.108 0.064 0.055 0.042 0.024 0.020 0.009 

eCV 40 20 21 30 22 37 39 43 67 38 47 25 

D4

Revised "All Lab Report" Page 3 / 6 
 

Round Robin XXIV Laboratory Results 

Total Lutein, μg/mL Total Zeaxanthin, μg/mL Total Lutein&Zeaxanthin, μg/mL 

Lab 160 161 162 163 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 0.073 0.093 0.047 0.049 

FSV-BI 0.055 0.079 0.045 0.039 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.030 0.045 0.029 0.020 

FSV-BO 

FSV-BP 

FSV-BS 

FSV-BX 0.062 0.081 0.048 0.045 

FSV-BY 0.067 0.086 0.053 0.045 

FSV-CA 

FSV-CB 

FSV-CH 

FSV-CJ 0.109 0.138 0.081 0.068 

FSV-CK 0.174 0.196 0.107 0.152 

FSV-CL 

FSV-CM 

FSV-CO 

FSV-CP 

FSV-CQ 

FSV-CS 

FSV-CT nd 0.182 0.114 0.310 

FSV-CU 

FSV-CV 

FSV-CY 

FSV-DC 

FSV-DE 

FSV-DL 

FSV-DM 

FSV-DS 

FSV-DW 0.045 0.043 0.026 0.027 

FSV-DY 0.091 0.147 0.082 0.093 

FSV-EA 

FSV-EB 

FSV-EC 

FSV-EF 

FSV-EI 

FSV-EJ 

FSV-EN 

FSV-EV 

FSV-EY 

FSV-FM 

n 9 10 10 10 

Min 0.030 0.043 0.026 0.020 

Mean 0.078 0.109 0.063 0.085 

Max 0.174 0.196 0.114 0.310 

SD 0.043 0.054 0.031 0.088 

CV 25 27 27 28 

NISTa 

NISTb 0.078 0.080 0.051 0.043 

NISTc 0.067 0.078 0.047 0.039 

Median 0.067 0.090 0.051 0.047 

eSD 0.033 0.067 0.034 0.030 

eCV 49 75 68 65 

160 161 162 163 

0.019 0.027 0.019 0.021 

0.010 0.022 0.013 0.012 

0.011 0.021 0.015 0.011 

0.015 0.021 0.015 0.015 

nd 0.070 0.040 0.091 

160 161 162 163 

0.127 0.166 0.098 0.085 

0.092 0.120 0.066 0.070 

0.080 0.110 0.074 0.065 

0.057 0.076 0.050 0.050 

0.077 0.102 0.063 0.060 

0.095 0.131 0.077 0.067 

nd 0.252 0.154 0.401 

4 5 5 5 

0.010 0.021 0.013 0.011 

0.014 0.032 0.020 0.030 

0.019 0.070 0.040 0.091 

0.004 0.021 0.011 0.034 

22 30 28 38 

0.053 0.041 0.033 0.033 

0.023 0.030 0.019 0.017 

0.013 0.022 0.015 0.015 

0.004 0.001 0.003 0.006 

29 7 20 40 

D5

6 7 7 7 

0.057 0.076 0.050 0.050 

0.088 0.137 0.083 0.114 

0.127 0.252 0.154 0.401 

0.023 0.058 0.035 0.127 

18 23 22 32 

0.131 0.121 0.084 0.076 

0.090 0.108 0.066 0.056 

0.086 0.120 0.074 0.067 

0.014 0.027 0.016 0.010 

16 22 22 15 

Revised "All Lab Report" Page 4 / 6 
Round Robin XXIV Laboratory Results 

Legend
 

nd Not detected (i.e., not reported or reported as '0', 'not determined', etc.)
 

<x Value less than x
 

! Invalid sample, reason unknown
 

italics Value calculated from reported results
 

n Number of non-NIST laboratories reporting quantitative results
 

Min Minimum non-NIST reported value.
 

Mean Average over all non-NIST reported values.
 

Max Maximum non-NIST reported value.
 

SD Standard deviation over all non-NIST values.
 

CV Coefficient of Variation (% relative standard deviation): 100*SD/Mean
 

Median Median over all non-NIST reported values 

eSD Robust estimate of SD based on the adjusted median absolute difference from the median (MADe) 

eCV Robust estimate of CV, 100*eSD/Median 

D6
 

Revised "All Lab Report" Page 5 / 6 
 

 

Round Robin XXIV Laboratory Results 

% Bias Summary 

Lab TR aT g/bT bC 

FSV-BA -2±1 2±2 1±1 2±3 

FSV-BD 0±4 -3±4 

FSV-BE -8±4 -23±7 

FSV-BF 8±6 1±3 -6±10 19±17 

FSV-BG -7±2 -13±3 -15±26 

FSV-BH -9±4 -13±1 -7±3 2±10 

FSV-BI -3±2 -4±4 2±3 -5±6 

FSV-BJ -2±3 -3±4 10±5 15±8 

FSV-BK 2±2 0±2 

FSV-BL 4±6 11±10 

FSV-BM -3±2 -1±2 

FSV-BN 4±5 12±4 -9±4 3±16 

FSV-BO 19±6 22±9 -17±13 

FSV-BP 17±15 21±5 23±23 

FSV-BS 34±14 40±64 

FSV-BX -1±5 

FSV-BY -1±5 1±2 7±5 11±6 

FSV-CA 4±3 8±3 

FSV-CB -21±5 -4±4 

FSV-CH 12±4 7±10 20±16 

FSV-CJ 11±7 5±4 1±4 

FSV-CK 11±17 9±17 22±17 -21±18 

FSV-CL 12±9 6±2 -67±1 -19±9 

FSV-CM 0±4 

FSV-CO -5±1 -1±1 13±7 

FSV-CP -12±2 

FSV-CQ -15±2 12±6 46±38 

FSV-CS 3±2 

FSV-CT 5±69 51±62 

FSV-CU -6±3 -1±3 1±3 

FSV-CV 0±1 -4±2 6±3 1±25 

FSV-CY 7±4 -2±2 -1±15 

FSV-DC 4±2 7±5 15±7 11±14 

FSV-DE 0±2 -2±2 

FSV-DL -2±4 -4±7 

FSV-DM 25±6 -22±4 13±47 

FSV-DS -13±10 -17±3 -28±2 

FSV-DW -60±3 

FSV-DY -4±4 16±19 -12±8 

FSV-EA -1±3 10±10 

FSV-EB 2±3 -2±1 9±7 

FSV-EC 0±3 9±7 10±23 

FSV-EF -5±7 1±3 9±13 

FSV-EI -10±7 -14±3 -12±7 -40±15 

FSV-EJ 7±8 -7±4 1±13 -22±45 

FSV-EN -42±9 -34±11 -30±7 

FSV-EV 3±3 6±4 

FSV-EY 6±6 10±3 

FSV-FM -5±1 -1±6 2±11 

NISTa -10±4 -6±4 0±4 7±6 

NISTb -13±3 8±3 1±3 -9±14 

NISTc -2±2 4±3 -13±7 -4±5 

Label Definition 

Lab Participant code 

TR Total Retinol 

aT a-Tocopherol 

g/bT g/b-Tocopherol 

bC Total b-Carotene 

% Bias (Mean ± SD) of individual serum biases 

Mean Average of (xi

-Mediani)/Mediani 

SD Standard deviation of (xi

-Mediani)/Mediani 

xi Result for analyte in serumi 

Mediani Median of non-NIST results in serumi 

The original analysis listed % Bias for each result for 

each serum calculated relative to the "Trimmed Core 

Lab Average" of that analyte in the serum. The 

summary values reported here are the (arithmetic mean 

± standard deviation) of each laboratory's reported 

results for the analyte estimated relative to each 

serum's median value. 

D7
 

Revised "All Lab Report" Page 6 / 6 
 

 

 

 

Appendix E. Shipping Package Inserts for RR25 

Two items were included in each package shipped to an RR25 participant: 

•	 Cover letter. The original letter has been lost. It likely would have described the four 

sample materials (sera 164 thru 167), given guidance on reconstituting these lyophilized 

samples, stated that results were due June 26, 1992 and to whom they should be sent, and 

who to contact with technical or programmatic questions. 

•	 Datasheet. The following page reproduces the form. 

These items were attached to the shipping box. 

E1
 
 

 

 

 

 

 

ROUND ROBIN XXV RESULTS FROM LABORATORY # _________ 

DATE OF ANALYSIS _____________ 

RESULTS IN ug/mL 

SAMPLE # ANALYTE RESULT 

SERUM 164 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 165 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 166 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 167 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

OPTIONAL ANALYTES : SUPPLY ONE RESULT IF AVAILABLE 

SERUM # 164 165 166 167 

TRANS-BETA-CAROTENE ______ ______ ______ ______ 

ALPHA-CAROTENE ______ ______ ______ ______ 

RETINYL PALMITATE ______ ______ ______ ______ 

GAMMA-TOCOPHEROL ______ ______ ______ ______ 

LYCOPENE (TOTAL) ______ ______ ______ ______ 

9-CIS-BETA-CAROTENE ______ ______ ______ ______ 

13-CIS-BETA-CAROTENE ______ ______ ______ ______ 

LUTEIN ______ ______ ______ ______ 

ZEAXANTHIN ______ ______ ______ ______ 

BETA-CRYPTOXANTHIN ______ ______ ______ ______ 

RECONSTITUTE SERUM SAMPLES WITH 1.0 mL OF WATER. 

RESULTS DUE BY JUNE 26, 1992 

NIST FAX # 301-926 8671 

E2
 
 

 

 

Appendix F. Final Report for RR25 

The following seven pages are the final report for RR25 as provided to all participants: 

•	 A cover letter and discussion. 

•	 Tables 1 thru 4 that list the results and various summary values for total retinol, 

α-tocopherol, total β-carotene, and γ/β-tocopherol. 

•	 Tables 5 tthru 13 that list the results and simple summary statistics for 

trans-β-carotene, total α-carotene, retinyl palmitate, total lutein, total lycopene, 

total zeaxanthin, total lutein & zeaxanthin, total β-cryptoxanthin, and 

trans-lycopene,. 

Due to the complex formatting used in the Tables, the originally listed laboratory codes 

have been deleted without replacement. However, Appendix G provides a complete 

listing of the RR25 results where the original codes have been altered to ensure 

confidentiality. Appendix G also provides more relevant summary statistics. 

F1
 
F2
F

3
 

 

Appendix G. Updated “All-Lab Report” for RR25 

The following four pages are an updated version of an “All-Lab” report for RR25. This 

report has three parts: 

•	 pages 1 and 2 list results for all analytes reported by at least twice, counting both 

participants and NIST analysts. 

•	 page 3 l provides a legend for pages 1 and 2. 

•	 page 4 summarizes each participants’ performance for total retinol, α- and γ/βtocopherol, and total β-carotene. These summaries are compatible with the 

percent bias evaluation advice given in the RR25 Report. However, the current 

bias summaries are estimated relative to the median of all reported values for each 

analyte in each serum rather than to the “Trimmed Core Lab Average” used in the 

original and detailed in Appendix F. These original reference values were 

estimated from on-time results of the more experienced participants, with 

subjective exclusion of results deemed non-representative. 

To ensure confidentiality, the laboratory identifiers used in this “All-Lab Report” have 

been altered from those used in RR25. The only attributed results are those reported by 

NIST. The NIST results are not used in the assessment of the consensus summary results 

of the study. 

Note: The analyst designated NISTa in this updated All-Lab report is designated “NIST” 

in the Tables described in Appendix F. 

G1 
Round Robin XXV Laboratory Results 

Total Retinol Retinyl Palmitate α-Tocopherol γ/β-Tocopherol Total β-Carotene trans-β-Caroten

G

2

Lab 164 165 166 167 164 165 166 167 164 165 166 167 164 165 166 167 164 165 166 167 164 165 166 

FSV-BA 

0.824 0.506 0.186 0.999 0.065 0.033 0.003 0.083 9.47 9.39 6.78 4.92 0.78 2.54 0.83 1.60 2.050 0.999 0.197 0.240 1.920 0.187 0.935 

FSV-BD 0.910 0.516 0.190 1.114 9.13 9.62 6.36 4.77 

FSV-BE 0.968 0.511 0.188 1.047 10.50 9.62 5.74 4.58 0.90 2.50 0.85 1.45 1.736 1.105 0.146 0.249

FSV-BF 0.901 0.532 0.226 1.155 10.15 9.90 6.85 5.30 0.70 2.40 0.70 1.50 2.491 1.124 0.157 0.334

FSV-BG 0.071 nd nd nd 0.867 0.525 0.176 1.088 9.85 9.95 6.84 4.95 1.742 1.148 0.180 0.261

FSV-BH 

0.679 0.427 0.181 0.876 0.023 0.060 nd nd 9.21 9.08 6.53 4.45 0.71 2.73 0.84 1.63 1.984 1.055 0.185 0.273 1.860 0.178 0.991 

FSV-BI 0.092 nd nd nd 0.914 0.557 0.193 1.136 9.94 9.92 6.86 4.42 0.76 2.81 0.87 1.73 2.001 1.085 0.186 0.264

FSV-BJ 0.764 0.520 0.182 1.053 0.042 0.089 nd nd 11.01 9.15 6.24 4.98 1.01 2.91 1.13 1.75 1.980 1.119 0.197 0.251

FSV-BK 1.047 0.549 0.208 1.069 10.45 9.29 6.53 4.95 

FSV-BN 0.057 nd nd nd 

0.797 0.484 0.189 0.905 10.07 9.29 7.23 5.21 0.61 2.48 0.78 1.35 2.035 0.955 0.174 0.275 1.811 0.162 0.842 

FSV-BO 0.879 0.559 0.166 1.217 10.36 9.77 6.38 4.86 2.077 1.418 0.186 0.343

FSV-BP 0.936 0.620 0.283 1.108 12.94 10.87 5.68 15.74 1.502 1.612 0.386 0.294

FSV-BY 0.851 0.506 0.184 1.055 0.010 0.010 0.010 0.042 9.20 9.49 6.66 4.63 0.77 2.90 0.94 1.54 1.947 1.057 0.192 0.289

FSV-BZ 11.10 8.90 8.60 4.80 

FSV-CA 0.795 0.496 0.194 0.998 10.01 9.92 6.90 5.48 

FSV-CB 0.716 0.436 0.151 0.899 8.97 9.17 6.30 4.11 

FSV-CH 0.832 0.500 0.188 1.009 8.81 9.61 5.83 4.50 1.786 1.032 0.169 0.255

FSV-CJ 1.124 0.559 0.219 1.255 8.28 8.75 5.24 3.21 1.207 0.837 0.149 0.166

FSV-CM 9.00 9.20 6.50 4.10 

FSV-CO 0.787 0.514 0.165 0.990 9.22 8.98 6.70 4.63 2.087 0.993 0.197 0.282

FSV-CP 0.921 0.584 0.217 1.162 8.39 8.21 5.66 3.98 1.742 0.819 0.156 0.240

FSV-CQ 0.855 0.512 0.199 1.140 9.73 9.75 6.12 5.01 2.342 1.221 0.139 0.264

FSV-CT 2.356 0.945 0.193 0.261

FSV-CU 

0.853 0.507 0.197 1.024 0.037 0.040 0.087 nd 9.40 8.70 6.76 4.45 1.743 0.976 0.194 0.225 1.628 0.177 0.915 

FSV-CV 0.874 0.514 0.180 1.080 9.02 9.80 5.58 4.26 0.76 2.38 0.83 1.57 2.210 0.981 0.124 0.255

FSV-CY 0.870 0.540 0.180 1.130 8.91 8.83 5.52 4.78 2.380 1.160 0.250 0.400

FSV-DC 0.794 0.513 0.192 0.953 9.37 9.13 6.67 5.69 0.64 3.04 1.99 1.98 2.133 1.053 0.149 0.230

FSV-DL 0.970 0.564 0.201 1.120 10.08 9.14 5.97 4.78 2.030 0.495 0.128 0.195

FSV-DM 1.156 0.720 0.302 1.376 9.41 9.89 6.46 3.91 1.958 0.775 0.150 0.241

FSV-DS 1.007 0.703 0.331 1.058 10.53 9.19 7.15 5.49 1.382 0.755 <0.05 0.150

FSV-DY 0.827 0.535 0.221 1.073 1.960 0.885 0.169 0.232

FSV-EB 0.957 0.547 0.218 1.070 10.05 10.04 6.62 4.57 1.408 0.866 0.180 0.231

FSV-EC 0.961 0.556 0.201 1.179 11.42 11.20 7.56 5.96 2.882 1.316 0.218 0.357

FSV-EJ 0.861 0.697 0.148 0.858 10.29 9.45 6.32 4.15 5.31 3.09 7.05 1.78 2.402 1.218 0.176 0.299

FSV-EN 10.87 10.69 7.64 7.68 1.77 4.44 3.18 2.85 4.130 2.750 1.500 1.320

n 31 31 31 31 8 5 3 2 33 33 33 33 12 12 12 12 29 29 28 29 4 4 4 

Min 0.858 0.679 0.427 0.148 0.042 0.010 0.010 0.003 8.28 8.21 5.24 3.21 1.35 0.61 2.38 0.70 0.50 1.21 0.124 0.150 0.842 1.628 0.162 

Mean 1.071 0.887 0.542 0.202 0.073 0.035 0.028 0.007 9.70 9.82 6.67 4.83 1.73 1.23 2.85 1.67 1.09 2.06 0.230 0.299 0.921 1.805 0.176 

Max 1.376 1.156 0.720 0.331 0.092 0.065 0.040 0.010 15.74 12.94 10.87 7.68 2.85 5.31 4.44 7.05 2.75 4.13 1.500 1.320 0.991 1.920 0.187 

SD 0.111 0.106 0.066 0.040 0.018 0.021 0.016 0.005 1.27 0.91 1.01 0.77 0.39 1.32 0.56 1.84 0.38 0.54 0.254 0.203 0.062 0.126 0.010 

CV 8 9 9 12 20 32 39 49 8 7 9 10 14 25 13 26 14 13 17 15 6 7 6 

NISTa 0.99 0.862 0.516 0.173 9.55 9.53 6.48 4.45 1.97 0.70 2.69 0.72 1.06 1.56 0.206 0.221 0.961 1.350 0.183 

Median 1.070 0.870 0.525 0.192 0.077 0.037 0.033 0.007 9.37 9.80 6.53 4.78 1.62 0.76 2.77 0.86 1.05 2.00 0.180 0.261 0.925 1.836 0.178 

eSD 0.098 0.098 0.036 0.018 0.020 0.021 0.55 0.89 0.47 0.49 0.19 0.13 0.40 0.12 0.16 0.38 0.025 0.042

eCV 9 11 7 9 26 56 6 9 7 10 12 18 14 14 15 19 14 16 

Revised "All Lab Report" 
Round Robin XXV Laboratory Results 

Total α-Carotene Total Lycopene Total β-Cryptoxanthin Total Lutein Total Zeaxanthin 

G

3

Lab 164 165 166 167 164 165 166 167 164 165 166 167 164 165 166 167 164 165 166 167 1

FSV-BA 0.063 0.012 0.011 0.038 0.135 0.258 0.162 0.303 0.048 0.046 0.340 0.055 0

FSV-BD

FSV-BE 0.040 0.010 0.010 0.020 0.050 0.150 0.080 0.210 

FSV-BF 0.088 0.039 nd 0.032 0.162 0.256 0.218 0.330 

FSV-BG 0.026 0.034 nd nd 0.106 0.342 0.226 0.512 

FSV-BH 0.

0.057 0.009 0.012 0.031 0.136 0.272 0.180 0.333 0.058 0.084 0.061 0.096 0.056 0.084 0.041 0.077 0.015 0.028 0.014 0.034 

FSV-BI 0.063 0.016 0.016 0.032 0.113 0.201 0.140 0.246 0.046 0.056 0.034 0.067 0.054 0.101 0.044 0.092 0.019 0.037 0.022 0.039 0

FSV-BJ 0.039 0.012 0.015 0.023 0.070 0.142 0.085 0.163 

FSV-BK

FSV-BN 0.047 0.019 nd 0.016 0.111 0.160 0.122 0.161 0.034 0.029 0.017 0.037 0.033 0.100 0.055 nd 0.014 0.018 0.016 nd 0

FSV-BO 0.068 0.038 nd nd 0.115 0.262 0.262 0.183 0.049 0.073 0.040 0.095 0

FSV-BP 0.037 0.013 0.019 0.049 0.137 0.217 0.156 0.242 

FSV-BY 0.062 0.014 0.020 0.037 0.107 0.239 0.172 0.268 0.041 0.037 0.030 0.056 0.048 0.080 0.035 0.069 

FSV-BZ

FSV-CA

FSV-CB

FSV-CH

FSV-CJ 0.029 0.008 0.024 nd 0.119 0.227 0.124 0.282 0.037 0.047 0.024 0.065 0

FSV-CM

FSV-CO

FSV-CP 0.074 0.013 0.017 0.039 0.118 0.215 0.165 0.258 0.028 0.036 0.022 0.043 0

FSV-CQ

FSV-CT

FSV-CU

FSV-CV 0.064 0.010 0.018 0.028 0.100 0.182 0.157 0.206 

FSV-CY

FSV-DC

FSV-DL 0.048 0.011 0.011 0.028 0.215 0.130 0.075 0.126 0.033 0.066 0.026 0.050 0

FSV-DM

FSV-DS

FSV-DY 0.102 0.199 0.131 0.227 

FSV-EB

FSV-EC

FSV-EJ 0.069 0.016 0.020 0.041 0.215 0.220 0.206 0.338 

FSV-EN

n 16 16 12 13 17 17 17 17 9 9 9 9 4 4 4 3 3 3 3 2 

Min 0.019 0.026 0.008 0.010 0.126 0.050 0.130 0.075 0.037 0.028 0.029 0.017 0.055 0.033 0.080 0.035 0.016 0.014 0.018 0.014 0

Mean 0.033 0.055 0.012 0.017 0.258 0.124 0.216 0.157 0.063 0.042 0.053 0.066 0.073 0.048 0.091 0.040 0.030 0.016 0.028 0.018 0

Max 0.049 0.088 0.016 0.032 0.512 0.215 0.342 0.262 0.096 0.058 0.084 0.340 0.092 0.056 0.101 0.044 0.039 0.019 0.037 0.022 0

SD 0.008 0.017 0.003 0.006 0.091 0.043 0.054 0.052 0.021 0.010 0.019 0.104 0.015 0.010 0.011 0.005 0.012 0.003 0.010 0.006 0

CV 17 20 16 18 18 20 16 20 22 16 22 30 17 19 11 10 31 14 26 26 

NISTa

Median 0.033 0.060 0.012 0.016 0.246 0.115 0.217 0.157 0.056 0.041 0.047 0.030 0.073 0.051 0.092 0.041 0.034 0.015 0.028 0.018 0

eSD 0.008 0.018 0.003 0.006 0.085 0.022 0.058 0.049 0.016 0.010 0.016 0.012 0

eCV 25 30 25 37 34 19 27 31 29 25 35 40 

Revised "All Lab Report" 
Round Robin XXV Laboratory Results 

Analytes Reported By One Laboratory 

Values in μg/mL 

Analyte Code 164 165 166 167 

trans-Lycopene FSV-BA 0.157 0.076 0.136 0.078 

Legend 

nd Not detected (i.e., not reported or reported as '0', 'not determined', etc.)
 

italics Value calculated from reported results
 

n Number of non-NIST laboratories reporting quantitative results
 

Min Minimum non-NIST reported value.
 

Mean Average over all non-NIST reported values.
 

Max Maximum non-NIST reported value.
 

SD Standard deviation over all non-NIST values.
 

CV Coefficient of Variation (% relative standard deviation): 100*SD/Mean
 

Median Median over all non-NIST reported values 

eSD Robust estimate of SD based on the adjusted median absolute difference from 

the median (MADe) 

eCV Robust estimate of CV, 100*eSD/Median 

G4
 

Revised "All Lab Report" Page 3 / 4 
Round Robin XXV Laboratory Results
 

% Bias Summary 

Lab TR aT g/bT bC Label

-5±2 1±4 

FSV-BD 

FSV-BA 

1±3 -2±1 

FSV-BE 1±7 -2±8 

FSV-BF 8±7 6±4 

FSV-BG -2±4 4±2 

FSV-BH -16±7 -4±4 

FSV-BI 4±3 1±6 

FSV-BJ -5±5 2±8 

FSV-BK 8±9 2±3 

FSV-BN -8±6 5±5 

FSV-BO 2±12 2±4 

FSV-BP 19±20 46±25 

FSV-BY -3±1 -2±2 

FSV-BZ 10±18 

FSV-CA -5±4 7±6 

FSV-CB -18±2 -7±5 

FSV-CH -4±1 -6±4 

FSV-CJ 17±9 -19±10 

FSV-CM -6±6 

FSV-CO -8±5 -3±5 

FSV-CP 10±3 -14±3 

FSV-CQ 1±4 0±5 

FSV-CT 

FSV-CU -2±3 -4±7 

FSV-CV -2±3 -7±7 

FSV-CY 1±5 -8±7 

FSV-DC -5±5 4±11 

FSV-DL 7±3 -2±5 

FSV-DM 39±13 -5±9 

FSV-DS 30±32 7±7 

FSV-DY 3±9 

FSV-EB 7±6 2±5 

FSV-EC 8±3 19±4 

-3±4 -1±8 Lab 

TR 

-1±13 -8±11 aT

-12±5 11±19 g/bT

-1±9 bC

-2±3 2±3 % Bias

2±3 2±2 

19±14 3±6 Mean

SD

-14±5 -2±6 xi

18±17 Mediani

39±60 

 Definition 

 Participant code 

 Total Retinol 

 a-Tocopherol 

 g/b-Tocopherol 

 Total b-Carotene 

 (Mean ± SD) of individual serum biases 

 Average of (xi-Mediani)/Mediani 

 Standard deviation of (xi

-Mediani)/Mediani 

 Result for analyte in serumi 

 Median of non-NIST results in serumi 

2±6 4±6 The original analysis listed % Bias for each result for 

each serum calculated relative to the "Trimmed Core 

Lab Average" of that analyte in the serum. The 

summary values reported here are the (arithmetic mean 

-5±4 ± standard deviation) of each laboratory's reported 

-29±11 results for the analyte estimated relative to each 

serum's median value. 

4±7 

-14±6 

3±18 

3±11 

-7±10 

-5±6 -8±17 

30±20 

37±65 -6±11 

-27±22 

-13±10 

-34±7 

-9±6 

-15±13 

31±10 

FSV-EJ -3±26 -3±9 334±377 12±10 

FSV-EN 26±23 135±95 351±286 

NISTa -5±4 -2±4 -1±16 -6±17 

G5
 

Revised "All Lab Report" Page 4 / 4 
 

 

 

 

 

 

Appendix H. Shipping Package Inserts for RR26 

Two items were included in each package shipped to an RR26 participant: 

•	 Cover letter. The original letter has been lost. It likely would have described the three 

lyophilized (sera 168 thru 170) and two liquid-frozen (sera 171 and 172) sample 

materials, given guidance on reconstituting the lyophilized samples, stated that results 

were due October 16, 1992 and to whom they should be sent, and who to contact with 

technical questions. 

•	 Datasheet. The following page reproduces the form. 

These items were attached to the shipping box. 

H1
 
 

 

 

 

 

 

 

ROUND ROBIN XXVI RESULTS FROM LABORATORY # _________ 

DATE OF ANALYSIS _____________ 

RESULTS IN ug/mL 

SAMPLE # ANALYTE RESULT 

SERUM 168 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 169 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 170 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 171 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

SERUM 172 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE (TOTAL) _____________ 

OPTIONAL ANALYTES : SUPPLY ONE RESULT IF AVAILABLE 

SERUM # 168 169 170 171 172 

TRANS-BETA-CAROTENE ______ ______ ______ ______ ______ 

ALPHA-CAROTENE ______ ______ ______ ______ ______ 

RETINYL PALMITATE ______ ______ ______ ______ ______ 

GAMMA-TOCOPHEROL ______ ______ ______ ______ ______ 

LYCOPENE (TOTAL) ______ ______ ______ ______ ______ 

9-CIS-BETA-CAROTENE ______ ______ ______ ______ ______ 

13-CIS-BETA-CAROTENE ______ ______ ______ ______ ______ 

LUTEIN ______ ______ ______ ______ ______ 

ZEAXANTHIN ______ ______ ______ ______ ______ 

BETA-CRYPTOXANTHIN ______ ______ ______ ______ ______ 

RECONSTITUTE SERUM SAMPLE NUMBERS 170, 171, 172 WITH 1.0 mL OF WATER. 

RESULTS DUE BY OCTOBER 16, 1992. 

NIST FAX # 301-926 8671 

H2
 
 

 

 

 

Appendix I. Final Report for RR26 

The following 16 pages are the final report for RR26 as provided to all participants: 

•	 The “Summary of 1992 Round Robin Activities” that was sent to participants in 

November 1992. 

•	 Tables 1a and 1b that summarize results for total retinol, α-tocopherol, and total 

β-carotene for the six Round Robin studies conducted from 1991 through 1992. 

•	 Tables 4 thru 7 that list the results and various summary values for total retinol, 

α-tocopherol, total β-carotene, and γ/β-tocopherol. Note: Tables 2 and 3 

reiterated the results provided in the RR24 and RR25 Final Reports and so are not 

included here. 

•	 Tables 8 thru 16 that list the results and simple summary statistics for 

trans-β-carotene, total α-carotene, retinyl palmitate, total lutein, total lycopene, 

total zeaxanthin, total lutein & zeaxanthin, total β-cryptoxanthin, and translycopene. 

•	 Six graphical presentations of “Interlaboratory Precision vs Time” for total 

retinol, α-tocopherol, and total β-carotene. Three of the Figures display the 

precision estimated from the “core laboratory” (laboratories that participated in 

previous round robin studies) measurements; the other three display precision 

estimated after trimming results considered to be distributional outliers. 

Due to the complex formatting used in the Tables 4 thru 16, the originally listed 

laboratory codes have been deleted without replacement. However, Appendix J provides 

a complete listing of the RR26 results where the original codes have been altered to 

ensure confidentiality. Appendix J also provides more relevant summary statistics. 

I1
 
c 

( 

SUMMARY OF 1992 ROUND ROBIN ACTIVITIES 

This report describes both overall-group and individual laboratory performance in the three 

Round-Robin exercises conducted during 1992. Specifically, this section contains, for retinol, 

a-tocopherol, and ~-carotene, respectively: both core and trimmed graphical information 

concerning Interlaboratory Precision vs Time over the past 6 1/2 years; for historical purposes, 

a summary table is also provided for data collected over the past two years; tabular presentations 

of both individual laboratory and summary statistical data for Round Robins XXIV, :XXV and 

XXVI; a Blind Control Chart representing a summary of each laboratory's data vs assigned 

values for the past five years; a graphical presentation of data from each laboratory's analysis of 

blind replicate samples over the past two years. Tabular data only are provided for a-carotene, 

trans ~-carotene, ~-cryptoxanthin, lutein, lycopene, retinyl palmitate, y-tocopherol and zeaxanthin. 

Table 1 provides a summary of interlaboratory data for retinol, a-tocopherol and ~-carotene over 

the past two years. The mean relative standard deviation (RSD; standard deviation expressed as 

a % ) for retinol Core Laboratories (Laboratories that had been involved in the Quality Assurance 

(QA) program for at least one year prior to Round-Robin :XXI) has averaged 10.7% over the past 

six Round Robin exercises with a range of 8.7-12.7%. New Laboratory RSD values have 

decreased steadily from approximately 65% in Round Robin XXII to values indistinguishable 

from Core Lab values in the past two studies. 

The mean RSD for a-tocopherol of Core Laboratories has averaged 9.6% with a range of 8.6-

10.6% over the past six Round Robin exercises. During the same period, New Laboratory RSD 

values have decreased from 54% in Round Robin XXII to approximately 20% in Round Robin's 

XXIII-XV, and to less than 10% in Round Robin XXVI. 

The mean RSD for ~-carotene of Core Laboratories (using data for all sera with concentrations 

higher than 200 ng/mL) averaged 24% during 1991 and was reduced to 18% during 1992. The 

New Laboratory mean RSD during this period was 41 % with a range between 17% (for RR 

XXVI) and 82% showing no particular trend. 

Tables 2 and 3 provide a listing and statistical summary of data submitted in Round Robins 

XXIV and XXV respectively, for retinol (42 labs), a-tocopherol (41 labs) and ~-carotene (33 

labs). The "Core Lab Trimmed Averages" were used as Assigned Values for these samples. 

Five Serum samples (168-172) were distributed for analysis in Round Robin XXVI. Samples 168 

and 169 were liquid samples and 170-172 were lyophilized. Sera 170 and 172 were blind 

duplicates. Table 4 provides a summary of data submitted for retinol. Thirty-three labs submitted 

data: 26 "Core Labs" and 7 "New Labs" -- 3 participating for the fifth time and 4 participating 

for the third time. Data for use in evaluating laboratory performance is provided to the right side 

of the Table. The "Core Lab" Trimmed Values were used as the assigned values. By 

convention, 0-5% bias from the assigned value represents EXCEPTIONAL performance, 6-10% 

ACCEPT ABLE performance, 11-20% MARGINAL performance and >20% POOR performance 

relative to the current state of the art. 

I2
 
Tables 5 and 6 provide Round Robin XXVI data for cx-tocopherol and 13-total carotene 

respectively. Thirty-five labs submitted data for cx-tocopherol; 28 "Core Labs" and 7 "New 

Labs". Thirty labs submitted data for total 13-carotene; 23 "Core Labs" and 7 "New Labs". The 

erratic nature of the data being reported for 13-carotene continues to cause us concern. Therefore 

we have initiated extensive laboratory investigations focused on problems associated with the 

extraction and HPLC analysis of carotenoid compounds, with special emphasis on 13-carotene. 

The results from some of those studies are presented later in this report. 

Tables 7-16 provide summaries of data reported in Round Robin XXVI for other fat-soluble 

vitamin and carotenoid compounds. During the coming year, special efforts will be made to 

improve the measurement quality of retinyl palmitate and additional carotenoid compounds. 

If labs have concerns regarding their performance or a lab was rated "U"" based on the convention 

stated above, we suggest that they obtain a unit of SRM 968a and analyze all three levels. If, 

with minor method modifications, their measured values do not agree with the certified values, 

they contact Dr. Neal E. Craft at 301/975-3111 for consultation. We are willing to provide inhouse consultation (at the labs expense) if need be, but have found that most problems can be 

solved via telephone conversations. 

For non-NCI funded labs, fees of $300 for US labs and $600 for non-US labs will be assessed 

for participating in the "Fat-Soluble Vitamins QA 1993" program. An invoice to that effect will 

be mailed to those laboratories. 

The 1993 QA Program will consist of three Round Robin exercises. The first set of samples will 

be distributed the week of January 25 with results due March 19; written feed back will be 

provided to labs by April 26. The second set of samples will be shipped the week of April 26 

with results due by June 14 and feedback to labs by July 26. The third set of samples will be 

shipped the week of July 26. Results will be due by August 30 so that we can discuss all three 

exercises at the Annual QA Workshop that is being planned for late September or early October. 

The actual date has not been set yet. Feedback to participants who are not able to attend the QA 

Workshop will be provided by November 15. 

I3
 
Table la 

ROUND ROBIN XXI ROUND ROBIN lOCll ROUND ROBIN XXlll 

AETINOI. RETINOL RE Tl NOL 

SERUM II SERUM II SERUM II SERUM 11 SERUM II SERUM II SERUM(// SERUM II SERUM (// SERUM (// SERUM (// 

144 145 148 147 148 149 150 155 156 157 159 

GRANO (34) 0963 0 504 0.276 GRAN0(44) 0.210 0.510 0680 GRAND (44) 0.53 1 0401 0980 0496 

RSO 16.1 15.8 18.1 23.1 RSC 42.8 33.0 382 RSO 15.0 14.8 158 17 8 

CORE (30) 0.1163 0494 0.520 0.281 CORE (31) 0.197 0.:i06 0.662 CO'lE (30) 0.538 0.402 1.004 0 506 

RSD 90 119 10.9 11 .0 RSD 18.5 118 99 RSD 122 102 130 99 

NEW NEW(12) 0245 0521 0729 NEW (14) 0514 03911 0925 0475 

RSD RSD 116.7 61.1 684 RSD 205 224 208 292 

ASSIGNED 0958 0490 0 .514 0262 ASSONED 0186 0489 0659 ASSIGNED 0536 0405 I 010 0506 

RSO 6.5 7.8 10.0 8.7 RSC 5.4 5.0 7.1 RSO 4.9 6.5 54 59 

PREVIOl.6 0.821 0485 0.515 0.259 PAEVlOUS PAEVlOUS 0489 

DATE 1.118 li9J 6i9J 1/!11 DATE DATE 1f.ll 

a - TOCCf'HERO.. a-TOCCf'HERO.. a-TOCCf'HERQ 

GRAND(35) 107 6118 6 .64 498 GRAND(44) 4.80 1052 1640 ORAND(44) 7.52 1001 630 1051 

RSO 8.0 82 11 .3 12.6 RSO 28.4 27.3 27:2 RSC 12.9 14.4 14.0 150 

CORE (33) 108 692 669 503 CORE (34) 4 79 1035 1632 CORE (32) 7 44 989 630 1069 

RSO 8.0 82 11.4 12.5 RSO 10.5 11.8 90 RSO 8.3 11 .8 9.6 8.4 NEW NEW(10) 4.82 11 .07 16 76 NEW(12) 7 71 1027 630 1005 RSD RSD 54.0 63 7 55B RSD II zo n. u. 

ASSIGNED 107 691 659 4118 ASSIGNED 480 10.50 1659 ASSONED 755 ID 16 628 10.50 

RSD 60 35 67 84 RSD 1 .3 3 .0 31 RSD 49 54 54 39 

PREVIOUS 105 668 666 483 PREVIOUS PREVIOUS 

DATE 1/111 1111> 5111> 1111> DATE DATE 10.5 

lf.ll 

b-CAAOTENE b-CAAOTENE b-CAROTENE 

GRANO (24) 0836 I 144 0236 0450 ORAND(33) 0275 0194 2362 ORAND(32) 0378 0823 0139 0898 

RSO 30.5 27.8 85.8 27.3 RSO 34.8 17.5 18.D RSC 52.7 29.8 198 38.0 

CORE (21) 0.887 1.151 0.211 0.457 CORE (23) 0.282 0.891 2339 CO'lE (20) 0348 0.804 0.089 0.856 

RSD 26.5 294 398 283 RSD 34.8 13.0 14.4 RSD 24.8 18.9 343 20.9 

NEW NEW(10) 02311 0898 2415 NEW(12) 0426 0854 0221 0965 

RSO RSD 31 .1 252 24.9 RSD 712 421 203 492 

ASSIGNED 0848 1 DB9 0195 0422 ASSIGNED 0260 0890 2338 ASSIGNED 0371 0822 0091 0879 

RSO 4.8 82 8.8 8.4 RSO 22.7 1.8 13 RSC 13.8 15.8 193 12.4 

PAEVIOt..6 0.786 1.034 0 .11111 0.408 PAEVlOUS PREVIOUS 0.890 

DATE 1.118 li9J 5i9J 1/!11 DATE DATE .Sf.ii 

I4
 
GRANO (42) 

ASO 

CORE (291 

RSD 

NEW(13) RSD 

ASSIGNED 

ASO 

PAEVIOl.6 

DATE 

GAAND(41) 

ASO 

CORE (30) 

ASO 

NEW(11) 

RSD 

ASSIGNED 

RSD 

PREVIOl.6 

DATE 

GAAND(33) 

ASO 

CORE (21) 

RSD NEW(12) RSD 

ASSIGNED 

ASO 

PREVIOl.6 

DATE 

ROUND ROBIN XXIV 

RETINQ 

SAMPLE II SAMPLE II SAMPLE II SAMPLE 11 

160 161 182 183 

1.002 

24.2 

1 012 

112 

1 069 

302 

I 019 

44 

1.0IO 

Ollf.11 

623 

15.6 

624 

14.0 

6.21 

21.0 

639 

51 

628 

08'91 

0100 

51 .2 

0098 

516 621 

21.0 

0090 

11.0 

0091 

08,91 

0.681 

15.0 

0678 

77 

0 703 

238 

0673 

69 

0659 

05,91 

0.288 

18.2 

0 293 .

70 

0282 

327 

0293 

70 

0.291 

OSSO 

a - TOCOPHEAOL 

1595 

108 

16 12 

7.4 

1541 

178 

1595 

65 

1659 

05,91 

461 

13.1 

463 

11 .9 

4 48 

320 

461 

67 

462 

05'90 

b-CAAOTENE 

2205 

32.9 

2.223 294 

1541 

178 

2212 

9.1 

2338 

05'91 

1016 

22.0 

1.092 

17.9 

4.48 

32.0 

1073 

711 

1145 

05'90 

0.387 

13.8 

0.388 

79 

0.393 

21.4 

0383 

8.7 

0 369 .

OUlll 

5.64 

12.11 

666 9.2 

5.55 

206 

566 

70 

664 

01Al8 

0183 

2UI 

0.195 

12.9 

5.55 

20.8 

0195 

12.11 

0202 

01Al8 

GRAN0(28) 

ASO 

CORE (23) 

RSD 

NEW (5) RSD 

ASSIGNED 

ASO 

PREVIOUS DATE 

GAAN0(30) 

ASO 

CORE (24) 

ASO 

NEW(61 RSD 

ASSIGNED 

RSD 

PAEVIOl.6 

DATE 

GAAN0(27) 

RSO 

COAE (21) 

RSD 

NEW(81 

RSD 

ASSIGNED 

ASO 

PREVIOUS 

DATE 

Table lb 

ROUND ROBIN XXV RETINCl. 

SAMPLE 11 SAMPLE II SAMPLE II SAMPLE II 

184 185 168 167 

1.074 

10.2 

1.078 

102 

1037 

13 t 

1085 

82 

1.()22 

07.at 

9.70 

13.3 

945 88 

10.81 

244 

938 56 

1139 

07Al8 

1087 

35.7 

0 9911 

17.3 

1.405 

622 

1023 

12.11 

1027 

07,68 

0.895 

11.5 

0 885 .

122 

0.865 

132 

0872 

8.1 

0.848 

OtSO 

0 546 .

12.2 

0.539 

11.5 

0560 

1110 

0525 

4.1 

0.515 

05.9(1 

a- TOCOPHEFO. 

1182 

11.0 

1159 

1.8 

10.68 

Ill 

959 

55 

982 

01AIO 

461 

13.I 

463 

11.9 

7.60 

222 

636 

72 

665 

05.90 

b-CAROTENE 

2.038 25.2 

1.999 

13.6 

2.247 

'442 2030 

tt.7 

t .976 

OtAIO 

\ 

0226 

113 

0.172 

168 

0415 

131 

0169 

14.0 

0189 

05.90 

0202 

20.2 

0.197 

14.9 

0224 

352 

0194 

83 

018(, 

05,91 

564 

12.9 

566 

92 

551 

218 

466 

68 

4.lo 

05'91 

0300 

119.7 

0.264 

166 

0435 

101 

0256 

8.2 

05'91 

GRAND (33) 

ASO 

CORE ('-"" 

RSD 

NEW(7) RSD 

ASSIGNED 

RSO 

PRE\llOl6 

DATE 

GAAN0(35) 

RSO 

CORE (28) 

ASO 

NEW (7) 

RSD 

ASSIGNED 

RSD 

PREVIOl.6 

DATE 

GAAND(30) 

ASO 

CORE (23) 

RSD 

NEW (7) 

RSD 

ASSIGNED 

ASD 

PREVIOUS 

DATE 

ROUND ROBIN XXVI 

RETINCl. 

SAMPLE 11 SAMPLE 11 SAMPLE 11 SAMPLE II SAMPLE II 

188 169 170 171 172 

0 549 .

10.8 

0 548 .

11 .6 

0559 

79 

0546 

4.8 

0.553 

tOSO 

10.59 

9.8 

1041 

87 

1124 

116 

1033 

46 

1046 

1(),9() 

t.662 

17.11 

t .710 

156 

t .518 

23.9 

1716 

9.0 

1.618 

1(),9() 

0644 

10.7 

0.844 

12.t 

0648 

47 

0639 

7.3 

0.627 

10.9(1 

0669 

67 

0666 

66 

0680 

72 

0657 

52 

a - TOCOPHEAOL 

982 

8.3 

985 

8.8 

1170 

66 

983 

51 

966 

10AIO 

625 

10.1 

621 

10.3 

6 39 

97 

623 

69 

b-CAAOTENE 

0439 

22.2 

0.447 

239 

0.415 

14.6 

0456 

14.3 

0441 

10'90 

0621 

17.5 

0842 

17.4 

0553 

124 

0617 

11 .9 

0547 

70 

0.547 

67 

0548 

87 

0538 

49 

496 

11 .5 

4.93 

12.1 

506 95 

603 

97 

0400 

18.8 

0418 

146 

0348 

17.3 

0416 

14.8 

0 670 

68 

0667 

67 

0680 

75 

0662 

56 

618 

9.6 

613 

97 

6 39 

92 

613 

68 

0609 

16.4 

0.823 

15.3 

0.564 

193 

0588 

89 

I5
 
Table 4 

RO!a>d Robin XICVJ 

ltetinol ltHUlta X Bias frat Tr tl'lled Core \.ID Aver .... 

Sor\1111 S.r\1111 ,.....,, ,..,.,. Se"'"' Ser\1111 Ser\1111 _..,, Se"'"' Ser\1111 l lbt 161 169 170 171 1n le. 16& 169 170 171 tn 

0.551 

0

0.6311 0.615 0.562 0.6114 0.9 ·0. 2 4.2 4.5 3.3 . 517 0,601 0.606 o.sos 0.617 ·5.] ·6.0 ·7.1 0. 576 ·6.1 ·6.1 

0

0. 661 0.670 • 0.609 0.692 5.5 ].4 1.9 ll.3 4,5 . 541 0.652 0.652 o.sn 0.665 .. 0 .480 0.573 0.602 · 0.9 2.0 ·0.1 6.4 0.4 0. 504 0.596 0 • 12. 1 · 10.4 ·1.4 ·6.3 ·10.0 .513 0.591 0.634 o.soa 0.627 ·6.0 ·7.5 · 3.6 · 5.6 ·S,.4 

• 0

0.554 0.633 0.666 0.536 0.671 1.S ·1.0 1.] ·0.] 1.J .461 0.544 0.611 0.491 0.637 0.565 0.705 ·15.2 · 14.9 ·6.0 ·1.7 -3.a • 0.762 0.593 0.676 

0.596 l.5 10. 3 15.9 10,3 2.1 

0. 495 

0.

0.621 

733 0. 705 0.57a 0.617 9.2 14,7 7.2 7.5 3.1 0.643 0.5U 0.665 

0.539 ·9.3 ·2.9 · 2. 2 ·2.7 0.4 0."29 0.649 0.533 0.645 0 · 1.l ·1.6 · 1.l · 0.9 ·2.6 

0.574 

.570 0.616 0.661 0.550 0.666 4.4 · 3.6 1.6 2.3 0.6 0.662 0.647 0.526 0.653 5.2 3.6 ·1.6 0.550 · 2.2 ·1.4 

• 0. 409 

0.620 0.610 0.550 0.620 o.a ·l.O ·7.2 2.J -6.4 • 0.482 0. 695 0.5)4 0. 723 ·ZS. I · 24.6 5.7 ·0.7 9.2 0.525 0.606 0.680 0.542 o.m 

0.556 ·3.a ·5.2 ].4 o.a 11.0 0.632 0.641 0.541 o.m 1.9 · 1.1 ·1.4 1.9 ·9.5 • 0.613 

0

0.7Cl7 0.691 0.545 0.684 12.J 10. 6 5. 0 1.:s 3.2 . 516 0.6JS 0.6611 0.557 0.665 ·5.S · 0.7 1.6 l .6 0.4 0.5D 0.611 0.59' 0.49J 0.601 · 2.4 ·S. 3 ·9.6 ·1.3 ·1.9 0. 555 0.711 0.655 0.521 0.666 1.7 11.2 · 0.4 ·3.1 0.6 0.690 0.552 0.692 5.0 2.7 4.5 

0.5

0. 521 

45 • 0.675 

0.336 0. 719 • 0.617 o.•n ·4.6 ·47. 4 9.4 14.7 2.3 0.613 0. 546 0.709 ·0.2 5.6 J. 9 1.5 7.1 • 0.759 • 0.901 • 0.769 • 0.632 • 0.193 39. 1 41 . 0 17.0 17.5 19.1 0.630 0.671 0.770 0.630 0.767 15,4 6. 1 17 . 1 17.2 15.a 0.536 0.666 0.697 0.591 o.n1 7.4 4. 2 6.0 9.9 1,9 0.5

0

56 0.621 0.6U 0.555 0.661 1.9 · 2.9 l . 9 3.2 ·o.z . 525 0.631 0 .642 0.4"6 0.674 -:s.a · 0.2 ·2.l ·7.9 1.7 0.540 0,600 0.680 0.530 0.650 ·1.1 ·6.1 3.4 · 1.4 ·1.1 0.512 0.649 0.613 0.510 0.609 ·6.Z 1.5 ·6.1 ·5.2 ·a.o 0.566 0. 611 0.673 0.524 0.679 3.7 6.5 2.4 · 2.6 2.5 

WIST 0, 551 0. 664 0.6&1 0.514 0.121 

All lobe -- -·· • A c..r.. Lebo ··~ <15 ·101;26) \11; (JJ) 0.549 0.644 0.669 0.547 0.670 

so 

uo 

o.osa 0.069 0.045 0.038 0. 045 AVC 0.546 0.09 0.657 0.531 0.662 10.6 10.7 6.7 7.0 6.1 so 0.02' 0.047 0.034 0.027 0.037 

RSO 4. 6 7.3 5.2 4.9 5.6 eo .... llbe <15· 101;26> 

PUVIOUS AYC 0.546 0.644 0.666 0.547 0.667 VAU.t; 0.553 o.w SD 0.063 0.071 0.044 o.m 0.045 ISO 11.6 12. 1 6.6 6.7 6.7 

<•> ..... Lobtl105·110;:Sl • • Value r-for Core Lob Tr1med Averote. 

AVQ 0,591 0.655 0.717 0.59Z 0.716 101 • porttctpottn1 fOf' t"* fifth ti .... SD 0.<137 0.030 0.047 0.038 0.053 (b) • pert;cisa-ttn1 for the thfrd t i .. ~ ISO 6.l 4. 6 6.5 6.l 7. 4 

( b) ..... lobt(116·120;4> ee 170 Ind 172 .,.. tile - s.re. 

•llC 0.516 0.64Z 0.6SZ 0.515 0.6$1 

so 0.CIZ3 o.m 0.031 0.015 o.m 

ISO '.:s 5.Z 4.7 3.0 4.9 

---- ........ :: 

I6
 
Table 5 

Ro....:t RotJ In XXVI 

Alpha·TocOf>l>erol X Bi11 frost TrtlM*t Core Lab Aver•Q9. 

se....,,, Ser U'llllf Serl.lllll Ser~ S.Nllf ,.,,.., Lebt Str- .. ,,.. S.runl knml 168 169 170 171 1n Labl 168 169 170 171 172 

10.0ol 9.42 6.12 5.06 6.17 . z .a ·4.Z · 1.7 0.5 0.6 10.05 9.49 5.93 4.82 5.94 ·2.7 ·3.5 ·4.8 ·4.3 11.02 · 3.2 

10.41 

10.09 6.35 5.44 6.55 6.7 2.7 2.0 8.1 6.7 

9.47 

9.64 6.74 5.96 6.72 0.8 · 1.9 8.2 18.4 9.5 9.17 6.08 5.00 5.96 ·8.3 ·6.7 ·2.4 ·0.7 ·2.8 9.98 9.34 5.53 4.55 5.37 9.80 ·3.4 ·5.0 · 11.3 ·9.7 · 12.5 10.50 6.70 5.30 6.40 ·5 .1 6.8 7.6 5.l 4.3 

10.53 

10.411 10.06 7.02 5.31 6.71 1.5 2.3 12.7 5.5 10.5 10.39 6.94 4.90 6.21 2.0 5.7 11.5 ·2.7 1.2 10.59 9.92 5.92 4.40 5.51 2.5 0.9 ·4.9 . 12.6 · 9.9 10.10 9.59 • 7.55 6.0] • 7 .15 · 2.2 ·2.4 21.3 19.8 16.6 10.]9 10.00 6.31. 5.20 6.32 0.6 1.7 1.3 3.3 3.0 10.92 9.15 6.37 4.95 6.08 5.7 ·6.9 2.3 ·1.7 ·0.9 11. 07 10.55 6.36 4.88 6.28 7.2 7.3 2.1 ·3.1 2.4 • 11.50 • 11.00 7 .00 5.20 6.90 11.4 11.9 12.4 3.3 1Z.5 9.37 8.84 5.91 4.87 5.78 ·9.J • 10. 1 ·S. 1 · 3.3 ·5.8 10.42 9.73 5.81 4.16 6.10 0.9 ·1.0 ·6.7 · 17 .4 · 0.6 • 12.20 10.34 • 7.24 5.95 • 7.D 1a.1 5.2 16.3 18.2 19.5 10.91 10.56 6.15 5.05 6.25 5.6 7.5 · 1.2 0.2 I .9 10.25 9.87 5.115 4.61 5. 70 · 0.8 0.4 ·6. 1 ·8.5 ·7.1 10.60 9.56 6.74 s.so 6.74 2.6 ·2.7 8.2 9.2 9.9 10.26 9.60 5.97 4.99 5.92 ·0.6 ·2.4 ·4.1 ·1.0 ·3.4 • 7.64 • 7 .13 • 4.54 • 3.79 • 4.66 · 26.0 ·27.5 · 27.0 ·24.8 ·24.1 10.IO 10.61 6.06 4.68 6.04 4.6 a .a ·2.8 ·7 .1 ·1.6 5.71 4.54 5.64 · a.3 ·9.8 ·I. I 9.84 • 4.92 6. 15 5.il5 6.24 · 4.7 ·49.9 · 1.2 4.l 1.7 • 12.24 • 11.95 5.73 • 3.49 5.62 18.5 21.6 ·8.0 ·30.6 ·8.4 9.74 9.66 • 5.14 4.31 • 5. 14 ·5.7 ·1.8 · 17.4 ·14.J ·16.2 12.20 9.60 6.19 4.87 6.63 11.1 ·2. 3 · 0.6 · 3.3 I. I 11.24 9.62 6.72 5.28 6.28 8.8 ·2.1 7.9 4.9 2. 4 12.20 10.83 7 .17 5.74 7.14 18. 1 10.Z 15.1 14.0 16.4 12.90 9.44 7.,, 5.68 7 .11 24.9 ·3.1 14. 1 12.8 15.9 9. 13 8.6$ 5.68 4.58 5.70 ·11.6 ·12.0 ·a.a ·9.0 ·7.1 10.41 9. 86 6.09 4.71 5.91 0.8 0.3 ·Z.Z ·6.5 ·J.6 10.58 9.89 5.74 4.71 5.94 2.5 0.6 ·7.9 ·6.5 ·3.2 

NISI 10.0S 9.88 6.47 4.7a 6. 19 

All Labo 

AVG (35 ) 10.59 9.82 --··- 6.25 4.96 ·-· 6.1a tote Liile Trl.....i (15·101;24) so I .OJ 0.82 0.63 0.57 0.59 

RSO 9.8 8.] 10.1 11.5 9.6 AVG 10.33 9.113 6.23 5.03 6.13 

SD 0.48 0.50 0.43 0.49 0.41 Core Lib& (15·101;21) ISO 4.6 5.1 6.9 9.7 6.8 

A\IC 10.41 9.85 6.21 4.93 6.13 

SD 0.90 0.116 0.64 0.60 0.60 PREVlllJS 

RSI> 1.7 a.a 10.3 12.1 9.7 YAU£ 10.46 9.65 

<•> 11.-. Llba <105·110;3> 

* • Value- reiwwed for tore Lib Tr 1-.ed Aver1ae. AVG 11.88 10. 02 6.69 5.30 6.68 SD 0.55 0.70 0.49 0.44 0.43 <•l • perttctpettng tor the fifth tt11e. RSD 4.7 7.0 7.3 a.2 6.S (b) • participi11ting tor thll th i rd tiN. 

<bl »ew Lobe (116·120;41 · ... 170 8'1d m are th• saw Ser-•. 

AVG 10.76 9.46 6.15 4.92 6.17 

so 1.57 o.5a 0.66 0.51 0.64 RSD 14.6 6. 1 10.7 10. 4 10.4 

==·--·· ···----

I7
 
Table 6 

Ro..nd Rob in XlCVI 

Tota l Beta-C•rotene X at11 fran TrtMed core L.ab Awr a99. 

$eNlllll 

- Send Ser.,. Se""' Sennt Se.,.. Send 

l lbl 1611 169 170 171 172 l lbl 1611 169 170 

-

171 '*""" In 

1.664 0.436 0.668 0.461 0.6114 ·3.0 · 4 .4 11.3 10.8 16.4 

1 .633 0.412 0.540 0.361 0.549 ·4.8 ·9.7 · 12.5 · 13.2 · 6.6 

1.420 0.473 0.711 0.504 0.565 ·17.2 3.7 15.3 21.2 ·3.9 

1.819 0.500 0.626 0.389 0.591 6.0 9.6 1.5 ·6.5 0.6 

1.7Z7 0.453 0.593 0.408 0.583 0.7 · 0.7 · 3.9 ·1.9 ·0.8 • 2.221 0.548 • 0.996 0.525 • 0. 886 29.4 20.1 61.5 U..2 50.8 

1.490 • 0.102 o.n4 0. 374 0.699 · 13.2 · 77.6 17.4 ·10.1 18.9 

1. 9114 • 0.623 0.692 0.480 • 0.713 15.6 36.6 12.2 15.4 21.3 

1.7W 0.444 0.617 0.399 0.5611 4.7 1.7 o.o ·4.1 ·3.4 

1.570 0.425 0.545 0.376 0. 552 ·8.5 ·6.11 • '1.6 ·9.6 ·6.1 

1.760 0.381 0.626 0.408 0,602 2.6 · 16.5 1.5 ·1.9 2.4 

1.830 0.554 0.736 0. 471 0.621 6.7 21.5 19.3 13.Z 5.7 

1.890 0.470 o.sao 0.360 0.550 10.2 3,0 · 6.0 ·13,5 ·6.4 • 1.087 0.336 0.517 0.379 0.538 ·36.6 ·26.3 ·16. 2 · 11 .9 · 11.5 

1.876 0.489 0.658 0.425 0.6S1 9.3 7.2 6.7 2.2 10.8 

1.770 0.514 • 0.806 0.522 • 0.1117 3. 2 12.7 30.7 ZS.5 39.0 

1 .6S4 0. 417 0. 545 o.m 0. 498 · 3.6 ·8.6 · 11.6 ·9.1 -15.3 

I.SOS 0.373 0.5'0 0. 342 0. 567 · 12.3 ·111.2 ·10.9 -17.8 ·3.S • 1.276 0.371 0.673 0.455 0.651 ·25.6 ·111. 7 9. 1 9.4 10.8 

0.493 0.312 0.545 · 20.1 · 25.0 ·7.3 

1.580 • O.ZlO 0.5116 0.411 0.579 ·7.9 ·49.6 ·S.O -1.3 • 1.5 

1.780 0.4114 0.564 0.343 0.573 3.7 6.1 · 8.6 · 17.5 -2.5 • 2.149 0.566 0.710 0.485 • 0.136 25.2 24.1 15.1 16.6 25.2 

1.152 0.346 0.461 0.296 0.499 ·32.9 ·24.1 ·Z!l.3 · 28.8 • 15.1 

1.813 0.433 0.623 0.424 0.666 5.7 · 5.1 1. 0 1.9 13.3 

2.108 0.467 0.6111 0.2117 0.722 22.9 2.3 • 1.5 ·31.1 22.8 

1.085 0.495 0.541 0.377 0.549 ·36.8 11.5 · 12.3 ·9.5 ·6.7 

1.550 0.396 0.597 0.381 0.570 ·9.7 · 13.2 ·3.2 ·8.4 ·3.0 

1.576 0.43Z 0 .580 0.397 0.550 · 8. 1 ·5. 3 ·6.0 · 4.6 ·6.4 

1.345 0.333 0.459 0.275 0.389 ·21.6 · 27.0 ·25.6 ·31.9 ·3J.8 

NIST 1.S90 0.447 0.661 0.482 0.610 

All l.C. ·-··-·· Co,.., Lobe trloned <15· 101;23> 

AVJ: (30) 1.662 0.439 0.621 0.400 0.609 

so 0.298 0.097 0.109 0.066 0.100 AVG 1.716 0. 456 0.617 0.416 0.588 

ISO 17.9 22.2 17.5 16.6 16.4 so 0. 155 O.C65 0.074 0.061 0.052 

RSI) 9.0 14.3 11.9 14.6 8.9 

tor• l a t15·101;Zll 

AVG 1.710 0.447 0.642 0. 416 0.623 PREVlaJS 

so 0.266 o. 107 0.112 0.061 0.095 VALUE 1.618 0.441 

RSD 15.6 Z:S.9 17.4 14.6 1S.J 

(I) llew Lebo (108·114;31 • = val.,. re<ODW<f for Core l ab Tri- Average. 

AW 1.691 0.415 0.564 0.336 0.629 <•> = pert1c1pattna for the fifth th ... so 0.490 0.062 O.Oll9 0.077 o. 116 (b) • perticip•ting fc:1r the t·hfrd tif•. 

RIO 29.0 15.0 15.9 22.9 18.4 

5-l•• 170 ..i in .,.. tn. •- Ser•. 

(b) New l obe (116·120;4) 

AVJ: 1.3119 0.414 0.544 0.357 0.514 

so 0.227 0. 068 0.061 0.056 0.084 

ASO 16.4 16,4 11.3 15.6 16.4 

···- :a:~ .. 

I8
 
Table 7 Rol.l"IG Robin XXVJ 

G .... ·Toc~rol X I i•• f rOl'll Trisrn:d LID Aver-11e . 

SerUWlll 5en.d S.Md Sen.nll' ~ 

l All 1611 169 170 171 172 lAN 1611 169 170 171 172 

1. 5] 2.20 2 .25 2.28 2.27 9.1 · 8.2 8 .9 6.] 7.2 

1.411 2.Z3 2.05 2.oa 2.07 5.6 · 6.a · 0 .7 - 2.a · 2.2 

1.30 2. 11 2. 14 2 .00 2. 06 · 7 .2 ·11 .8 3 .7 · 6.6 ·2.7 

1.62 2.55 2.36 2.40 2. 28 15.6 6.6 14 . 3 12.1 1.1 

1.22 2 .91 2. 30 2.41 2.10 · 12.9 21 .7 11. 4 12.6 · 0.1 

1. 46 2.16 1.92 1.91 1.91 4.2 ·9.7 · 7.0 · 10.11 · 9.1 

1.29 1.85 1 ,79 1.79 1 .74 ·T.9 · 22. 6 ·13.l • 16. 4 • 17.1 

1.34 2.09 I. a! 1.43 • 2.76 ·4.4 ·12. 6 • 11 .3 • 14 .5 30.4 

1. 50 <.58 2.05 2.20 2. 11 7 .1 1.9 ·0. 5 2.a -o.s • 1 .96 2.96 • 2. 64 2.64 2. 62 39 .9 21.a 27.9 23.l 23.1 • I. al 3.03 2. 16 2.15 2. U 29. 2 26.7 4.7 0.4 4.9 

1. 27 2. 01 1.115 2. 00 1 .91 ·9.1 •15.0 · •0.2 ·6.6 -10. a 

""' 1. 482 2 .392 2. 112 2. 140 2.170 

so 0 .226 0.401 0.251 0 .257 0.291 

RSO 15 .2 16. 8 11.9 12 .0 13. 4 

S-lllPl•• 170 lr1d 1n • r• the .... k r 1. 

NIST 1 1.23 2 . 19 1.93 1.91 2. 17 

.isT l 1.51 Z.1.ti 2.02 2.03 1.88 

Tri....cl 

•VG 1.401 2.39Z ····- 2. 064 2.140 --2.11·

6 · 

so 0 .133 0 .401 o. 197 0 .:257 0.234 

RSO 9 .5 16.8 9.5 12.0 11.1 ..... _ • • velue l"tlnD"Hd for Tr t-0 Lib Average . ·-----

Table 8 ao.n1 lob in JONI 'lable9 - aob in JONI 

trans· let1 ·C1rotene Alph1·C&rotene 

serld ser..- Sor..., Sertml send 

-- serllllll SerUllll S1rU!lt Sand 

LAN 168 169 170 171 172 LAN 1611 169 170 171 172 

56 1.510 0 .392 0 . 512 0. 346 0.516 15 0 . 109 0 .062 0.024 0.015 0.025 

60 1.694 0 .365 0. 592 O.JM 0. 570 16 o.oaa o.osa 0 .021 0 .013 0.020 

92 1.6:ZS 0.343 0 .514 0.345 0 .47 1 19 0.063 0.042 0.020 0.013 0.019 

11 0 1.&48 0.369 0.620 o. ~ 0 .600 17 0.027 0 . 026 

32 0.115 0.079 0.052 o.on 

--····- . .....,..... 46 o.oaa 0.052 0 .044 0 .0 17 O.OZ9 

AVG 1.669 0.377 0. 560 0.376 0 . 5]9 56 0 .099 0.062 0.028 0 .013 0.029 

S1) 0 . 141 0.012 0 . 055 0.040 0.057 60 0 .098 0.049 0.022 0.013 0.022 

RSO a.s ].] 9.1 10.6 10.6 Tl 0.092 0.059 o.an 0 .021 0.029 

-·-- ·····- 116 O.OT2 0 .048 0 .011 0 .012 0.011 

&9 O.Oe6 0.056 0.026 0 .0 16 0.026 

NIST 1 1.450 0.403 0.591 0.352 0. 51!6 93 0 . 125 0.011 0.028 0 .016 0.029 

i>Wt'Wcts3 1.56 .388 .567 .382 .518 9S 0.019 0 .U1 1 0.020 97 0. 114 o.oaa O.Ol4 0.0}9 o.035 

VALUE 1.490 0 .401 1ca 0.066 0.047 0.016 0.013 o.ozo 

110 0.0711 0.048 0.02] 0 .012 o.ozs 

116 0 .067 0.053 0 .015 0.023 

--···-·· ====-... AVG 0 .087 0 .056 0 .026 0 .016 0.025 

SI> 0. 025 0.015 0.010 0. 007 o.~ 

uo 28.J 26. I 31.3 44.4 20.7 

--==-

NIST 1 o. 102 0 .057 o .aJ7 0 .017 O.OZ5 

NIST 3 .110 .066 .034 .027 .035 

I9
 
table LO Round Aobln XlCVI Table ll ROU"d Robln XXVJ 

Retinyl P• l• it• t• luie•n 

Str.- SerUlll se""" ~ Stt'lnlf Sc"""' se"""' Stnnil S.Nlil 

I.AU 111& 169 170 171 1n I.AN 16a 169 170 171 

-

172 

0.166 0.044 0.259 0.136 0.262 0.129 0.109 0.109 0.047 0.111 

o.m o.oas 0.372 o.2UT o.374 0.157 0.1"57 0.112 0.046 0.111 

0.223 0.045 0.312 0.201 0.270 0. 151 0.102 0.109 o.045 0.115 

0.220 0.076 0.302 o. 1114 0. 296 0.095 O.QI\ 0.075 0.031 o.on 

0. 160 o.o:sa 0.227 0.154 0.240 = =-- 0.247 0.094 0.296 0.193 o.za2 AW 0.133 0.1UT 0.101 0.042 0.10J 

0.375 0.158 0.474 o.330 0.471 SD o.oza 0.023 0.011 o.ooa o.ozo 0.237 0.064 0.317 0.222 0,352 uo 21.1 21.6 17.3 17.9 19.3 

···-- • 

AVG 0.241 0.074 0,3lQ 0.203 o •. 1ia 

so 0.070 0.039 0.075 0.051 0.017 MIS1 3 .145 .112 .uo .046 .105 

uo 29.0 52.0 ZJ.6 28.7 24.0 

·····- ···- NIST 3 .217 .059 .297 .185 .261 

l'lfVIOJS 

VALUE 0.192 O.C69 

Table 12 A....,., •.C. In UVl Table 13 •.....t ..C.ln llXVI 

~ z.u.nttlin 

seNllll St ..... 

- S.Nllf 

- ........ - StNllll .. ,,... ........ LA .. 161 169 170 171 172 LAIS 161 169 170 171 171 

0.340 0.311 0.231 0.202 0.242 0.038 0. 11'.M 0.043 0.023 0.04J 

0.294 0.290 0.169 o. 140 0.170 0.034 o.on 0.040 o.ozr 0.037 

0.3N 0.392 O.l64 0.3S4 0.221 0.017 0.011 O,OZJ 0.012 0.020 

0.270 0.265 0.188 o.1s8 0.190 • 

0,472 0.522 0.342 0.246 0.304 AVI; 0.030 0.029 0.035 0.021 o.o:n 

0.440 0,450 0.300 O.ZJO 0.270 so 0.011 0.010 0.011 o.ooa 0.012 

0.331 0.276 0.192 0.154 o. 183 uo 37.6 lS.3 30.5 37.6 n.a 

0.215 0.249 o. 183 0.175 o. 199 •• WWW 

0.187 0. 186 0.123 0.101 o. 124 11ST l .041 • 040 .051 .026 .048 

0.362 0.3114 0.230 0, 196 0.222 

0.436 0.466 0.269 o.zzo 0.286 

0.124 o. 101 0.145 

0.394 0.332 o.zn 0.196 0.237 

0.202 0.200 0.139 0.132 0. 155 

0.183 0. 170 o. 140 0.110 0. 124 

0.209 0.329 0.1112 0.159 0.199 

AVG 0.316 0.326 0.207 0.179 0.204 

·-- ······- so o. 101 0. 106 0.065 0.061 0.055 

uo 31.I 32.5 31. I 34.2 26.7 

····-- ••=--s 

MISI 3 .451 .422 .250 .225 '.234 

I10
 
I able Lii Round Robin XXVI iable LS Round Robin XXVI 

Lutein • 2e.tA9'1tfttn s.ta·Crypto...-.thin 

Ser'-"" SerU'Jlll: SerUI"# Sert.d SerU'llll SeN!'ll s ........ Se"""' Sen.mt Se.,.. 

LAii# 168 169 11a 171 172 LAU 168 169 170 171 1n 

0.1116 0.159 0.149 a.011 o. 151 0.118 a.099 a . 064 0.041 a.067 

a.212 0.182 a.182 0.080 0.1&9 0. 179 0.146 0.086 o.a51 0,087 

0.227 o. 1911 0. 1119 0.083 0.187 0.124 0.107 0.074 0.04S a.on 

0.341 0.263 o. 169 0.0111 0.1S7 o. 149 a.120 0.070 0.044 0.073 

0.158 0.071 o. 162 0.130 0.113 0.062 0.036 a.062 

0.126 o. 1a1 0.101 0.044 0.097 0.073 0.048 0.077 o. 124 0.249 o.zso 0.092 o.m 0.200 o. 150 a.100 0.058 0.09T 

··--··· ·--·· a.111 0.097 0.073 0.043 0.074 

AVG a.203 o. 193 a.168 0.074 a.168 o. 108 0.0&5 a .ass 0.032 0.059 

SD 0.079 a.058 a.040 0.015 a.042 0.067 o.1n 0.065 

RSO 39.1 30.0 23.6 20.4 24.9 :;::.....-

-- =- AllC 0.132 0. 122 0.072 a.044 0.074 

so 0.040 a.030 a.013 a.ooa a.OIZ 

RSO 30.1 24.6 11.a 17.5 16.0 

===---· NIST 3 .109 .087 .060 .034 0.054 

Table 16 ROlnl Robin XXVI 

Lycopene (TRAl!lll 

Ser.,.. Sel'\d Se ..... se,..,. Sel'\lltl 

LAU 168 169 170 171 1n 

0.214 0.213 a.134 a.111 0.134 

MIST 3 -. 180 . 166 .124 .106 .112 

I11
 
\ () 

lnterlaboratory Precision vs Time 

Core Laboratories 

Retinal 

40 I> • ---···· .. =._: ... ..... " :: ··••••·•·••• .. - -··- -. -- ... ·••••···••·· - ·: • • : : ::• •••••• ••·•· .... • •• /-· -· > .. -_ --- - I 

30 

ii 

20 : .'. . . . . .. . ... ........... .. .. . ... . •.. -. . . I! . . . . . . ' ; . .; . ; . -; ' . . . . . . . -. 

.... . ... 

-- ii 

.... ... .. 

101·· ······· ··· .·: · · ···Ill ··· .. Iii .... . .• • Ila ... ii .. .. .. .. .. . . . .. .. .. .. ... .. . . ... . : .. . .. : "" .. .. .. .. .. .. .. .. .. ... .. 

' lil bl 

3/86 10/86 4/87 7 /87 1 /88 7 /88 9/88 1 /89 4/89 8/89 1 /90 5/90 9/90 1 /91 5/91 8/91 1 /92 5/92 8/92 

I12
 
lnterlaboratory Precision vs Time 

Retlnol 

Core Labs Trimmed 

Percent 

30 

+ + + 

20 

+ 

+ 

10 ······ ····+·····*·· ·· +· ..... ... ..... .. . 

.. ....... ...... ++++ + + +++++ 

0 

IUfUD •fDI lff/16 lff/lf/I lff/lf/I •ffllf/I lffll• 

Date 

Controls Available 

+ % Retinal ( SD

I13
 
,.,.-.... ( ) ( . 

I . j 

lnterlatloratory Precision vs Time 

Core Laboratories 

Alpha-Tocopherol 

4o r .. .. . ·-. -- - . ..... ... ..... I 

i • •.• •· .. I 1•1 1•·••::: •1• : !11 1-1lll n : • · ... . . ···•·• ··•. •• ii . i iilirnll/i . ! ' Iii : ••••••. •.. . . ! . . ii ::i1m: Ill . : . . , • •. . •. .• • • . 

30 .... t .. . ;:: .. .. 

20 t·"""' ' ::::· . :··· ··· 

10 ,_ .. ....... o t :.:-! ·: "!' I ········ 1 ·· · . ······· ...... ... .......... .. .. ······ ··· ··· ···· ··········· ······ ·········· ·· ··· I ... .............. .... ············ . ········ ..... .. . . ·•··· ··· ···· ... .. ··· -·· ········ ······ ··· · .. . .. . .... ·- ... . ·· ·· ··· ...... .. ... ·········· ·· ····· .. ..... ····· . . . ....... . . 

0 

_

•///I ••. i Jiiiij/iiiij •;•!••• •1 • •:ll/l/![j ![I/I , ( L > i . • •n •• ••.. ::::;;;;; :)•ji ii!!'lllliif !JJll/1111 ••/ii rn l///i •l•I liiiiii llllilil i • ;· :::::• . :;; .:: •rn•: · [1[1/i i i .. ·. 

3/8610/864/87 7/87 1/88 7/88 9/88 1/89 4/89 8/89 1/90 5/90 9/90 1/91 5/91 8/91 1/92 5/92 8/92 

I 

I14
 
lnterlaboratory Precision vs Time 

Alpha-Tocopherol 

Core Labs Trimmed 

Percent 

30 

* 201* ..... * .... ... ... . - . .. . - .. - ... - - - - . - ... - .. - . - - - . - . . . . . - - . 

* 

10 *-- -- ---------

.. ****** * * * * * * * 

0 

D•t• 

Controls Available * % SD To

I15
 
n 

lnterlaboratory Precision vs Time 

Core Laboratories 

Total Beta-Carotene 

100 ......... I I · ..... 

ao········ 

60 

40 J> 

....... . 

0 I • :: .. · · · · .... · .. ::• •• • • •• ••:•:: : : • • ' :• : , /:: : / . : > ' ' > I 

3/8610/864/87 7/87 1/88 7/88 9/88 1/89 4/89 8/89 1/90 5/90 9/90 1/91 5/91 8/91 1/92 5/92 8/92 

I16
 
lnterlaboratory Precision vs Time 

Beta-Carotene 

Core Labs Trinuned 

Percent 

30 

x 

20 

x x x 

x x 

x x x x 

10 

- -- x x x- -x- -----x- -----

_____________ _____ z- _ x __ x 

x 

0 

Date 

Controls Available 

x % SD E-'1a-Carotene Bet

I17
 
 

 

 

 

Appendix J. Updated “All-Lab Report” for RR26 

The following five pages are an updated version of an “All-Lab” report for RR26. This 

report has three parts: 

•	 pages 1 thru 3 list results for all analytes reported by at least twice, counting both 

participants and NIST analysts. 

•	 page 4 lists values for all analytes reported by only once. This page also provides 

a legend for pages 1 thru 3. 

•	 page 5 summarizes each participants’ performance for total retinol, α- and γ/βtocopherol, and total β-carotene. These summaries are compatible with the 

percent bias evaluation advice given in the RR26 Report. However, the current 

bias summaries are estimated relative to the median of all reported values for each 

analyte in each serum rather than to the “Trimmed Core Lab Average” used in the 

original and detailed in Appendix J. These original reference values were 

estimated from on-time results of the more experienced participants, with 

subjective exclusion of results deemed non-representative. 

To ensure confidentiality, the laboratory identifiers used in this “All-Lab Report” have 

been altered from those used in RR26. The only attributed results are those reported by 

NIST. The NIST results are not used in the assessment of the consensus summary results 

of the study. 

Note: The analysts designated as NISTa and NISTb in this updated All-Lab report are 

designated as “NIST 1” and “NIST 3” in the Tables described in Appendix I. 

J1
 
 Round Robin XXVI Laboratory Results 

Total Retinol Retinyl Palmitate α-Tocopherol γ/β-Tocopherol Total β-Carotene 

Lab 

J2

FSV-BA
 

FSV-BD
 

FSV-BE
 

FSV-BF
 

FSV-BG
 

FSV-BH
 

FSV-BI
 

FSV-BJ
 

FSV-BK
 

FSV-BL
 

FSV-BN
 

FSV-BO
 

FSV-BP
 

FSV-BS
 

FSV-BT
 

FSV-BX
 

FSV-BY
 

FSV-BZ
 

FSV-CA
 

FSV-CB
 

FSV-CH
 

FSV-CJ
 

FSV-CM
 

FSV-CO
 

FSV-CP
 

FSV-CQ
 

FSV-CU
 

FSV-CV
 

FSV-CY
 

FSV-DC
 

FSV-DL
 

FSV-DM
 

FSV-DS
 

FSV-DY
 

FSV-EB
 

FSV-EC
 

FSV-EJ
 

168 169 170 171 172 168 169 170 171 172 168 169 170 171 172 168 169 170 171 172 168 169 170 171 1

0.539 0.629 0.649 0.533 0.645 

0.554 0.633 0.666 0.536 0.671 

0.596 0.733 0.705 0.578 0.687 

0.463 0.544 0.618 0.491 0.637 

0.576 0.661 0.670 0.609 0.692 

0.570 0.616 0.668 0.550 0.666 

0.517 0.601 0.606 0.505 0.617 

0.556 0.632 0.648 0.548 0.599 

0.613 0.707 0.691 0.545 0.684 

0.525 0.606 0.680 0.542 0.735 

0.556 0.621 0.683 0.555 0.661 

0.525 0.638 0.642 0.496 0.674 

0.586 0.666 0.697 0.591 0.721 

0.512 0.649 0.613 0.510 0.609 

0.574 0.662 0.647 0.526 0.653 

0.551 0.638 0.685 0.562 0.684 

0.480 0.573 0.602 0.504 0.596 

0.630 0.678 0.770 0.630 0.767 

0.521 0.336 0.719 0.617 0.677 

0.541 0.652 0.652 0.572 0.665 

0.513 0.591 0.634 0.508 0.627 

0.565 0.705 0.762 0.593 0.676 

0.533 0.618 0.594 0.493 0.603 

0.516 0.635 0.668 0.557 0.665 

0.550 0.620 0.610 0.550 0.620 

0.495 0.621 0.643 0.523 0.665 

na na 0.690 0.552 0.692 

0.759 0.901 0.769 0.632 0.793 

0.540 0.600 0.680 0.530 0.650 

0.409 0.482 0.695 0.534 0.723 

0.555 0.711 0.655 0.521 0.666 

0.566 0.681 0.673 0.524 0.679 

0.545 0.675 0.683 0.546 0.709 

0.220 0.076 0.302 0.184 0.296 

0.223 0.045 0.312 0.201 0.270 

0.160 0.038 0.227 0.154 0.240 

0.297 0.085 0.372 0.207 0.374 

0.247 0.084 0.296 0.193 0.282 

0.237 0.064 0.317 0.222 0.352 

0.166 0.044 0.259 0.136 0.262 

0.375 0.158 0.474 0.330 0.471 

10.39 10.00 6.31 5.20 6.32 

9.80 10.50 6.70 5.30 6.40

10.59 9.92 5.92 4.40 5.53 

10.48 10.06 7.02 5.31 6.78 

11.02 10.09 6.35 5.44 6.55 

10.92 9.15 6.37 4.95 6.08 

10.05 9.49 5.93 4.82 5.94 

10.91 10.56 6.15 5.05 6.25 

10.25 9.87 5.85 4.61 5.70

12.20 10.34 7.24 5.95 7.33

12.20 10.83 7.17 5.74 7.14 

12.90 9.46 7.11 5.68 7.11 

11.24 9.62 6.72 5.28 6.28 

10.41 9.86 6.09 4.71 5.91 

11.07 10.55 6.36 4.88 6.28 

10.04 9.42 6.12 5.06 6.17 

11.50 11.00 7.00 5.20 6.90 

9.47 9.17 6.08 5.00 5.96

12.20 9.60 6.19 4.87 6.63

9.84 4.92 6.15 5.25 6.24 

10.41 9.64 6.74 5.96 6.72 

10.42 9.73 5.81 4.16 6.10

9.98 9.34 5.53 4.55 5.37 

7.64 7.13 4.54 3.79 4.66 

10.53 10.39 6.94 4.90 6.21 

10.26 9.60 5.97 4.99 5.92 

10.60 9.56 6.74 5.50 6.74 

9.37 8.84 5.91 4.87 5.78 

10.10 9.59 7.55 6.03 7.15 

na na 5.71 4.54 5.64 

9.74 9.66 5.14 4.31 5.14 

9.13 8.65 5.68 4.58 5.70 

10.80 10.61 6.06 4.68 6.04 

10.58 9.89 5.74 4.71 5.94 

12.24 11.95 5.73 3.49 5.62 

1.46 2.16 1.92 1.91 1.91 

1.62 2.55 2.36 2.40 2.28 

1.30 2.11 2.14 2.00 2.06 

1.29 1.85 1.79 1.79 1.74 

1.48 2.23 2.05 2.08 2.07 

1.50 2.58 2.05 2.20 2.11 

1.27 2.03 1.85 2.00 1.91 

1.34 2.09 1.83 1.83 2.76

1.53 2.20 2.25 2.28 2.27 

1.96 2.96 2.64 2.64 2.62 

1.22 2.91 2.30 2.41 2.10 

1.81 3.03 2.16 2.15 2.22 

1.570 0.425 0.545 0.376 0.5

1.984 0.623 0.692 0.480 0.7

2.221 0.548 0.996 0.525 0.8

1.420 0.473 0.711 0.504 0.5

1.760 0.381 0.626 0.408 0.6

1.633 0.412 0.540 0.361 0.5

1.876 0.489 0.658 0.425 0.6

1.848 0.433 0.623 0.429 0.6

1.085 0.495 0.541 0.377 0.5

1.152 0.346 0.461 0.296 0.4

2.108 0.467 0.608 0.287 0.7

1.576 0.432 0.580 0.397 0.5

1.664 0.436 0.668 0.461 0.6

1.830 0.554 0.736 0.471 0.6

1.580 0.230 0.586 0.411 0.5

1.819 0.500 0.626 0.389 0.5

1.727 0.453 0.593 0.408 0.5

1.505 0.373 0.550 0.342 0.5

1.490 0.102 0.724 0.374 0.6

1.654 0.417 0.545 0.378 0.4

1.770 0.514 0.806 0.522 0.8

1.890 0.470 0.580 0.360 0.5

1.797 0.464 0.617 0.399 0.5

na na 0.493 0.312 0.5

2.149 0.566 0.710 0.485 0.7

1.550 0.396 0.597 0.381 0.5

1.087 0.336 0.517 0.379 0.5

1.276 0.371 0.673 0.455 0.6

1.345 0.333 0.459 0.275 0.3

1.780 0.484 0.564 0.343 0.5

n 32 32 33 33 33 8 8 8 8 8 34 34 35 35 35 12 12 12 12 12 29 29 30 30 

Min 0.409 0.336 0.594 0.491 0.596 0.160 0.038 0.227 0.136 0.240 7.64 4.92 4.54 3.49 4.66 1.22 1.85 1.79 1.79 1.74 1.085 0.102 0.459 0.275 0.3

Mean 0.548 0.635 0.669 0.547 0.670 0.241 0.074 0.320 0.203 0.318 10.57 9.68 6.25 4.96 6.18 1.48 2.39 2.11 2.14 2.17 1.660 0.432 0.621 0.400 0.6

Max 0.759 0.901 0.770 0.632 0.793 0.375 0.158 0.474 0.330 0.471 12.90 11.95 7.55 6.03 7.33 1.96 3.03 2.64 2.64 2.76 2.221 0.623 0.996 0.525 0.8

SD 0.058 0.087 0.045 0.038 0.045 0.070 0.039 0.075 0.058 0.077 1.03 1.16 0.63 0.57 0.59 0.23 0.40 0.25 0.26 0.29 0.294 0.103 0.109 0.067 0.1

CV 11 14 7 7 7 29 52 24 29 24 10 12 10 12 10 15 17 12 12 13 18 24 18 17 

NISTa
 

NISTb
 

0.551 0.664 0.688 0.514 0.721 

0.719 0.738 0.785 0.647 0.747 0.244 0.065 0.328 0.204 0.288 

10.05 9.88 6.47 4.78 6.19 

9.60 8.25 5.40 4.31 5.01 

1.23 2.19 1.93 1.91 2.17 

1.36 2.03 1.85 1.85 1.71 

1.590 0.447 0.661 0.482 0.6

1.660 0.415 0.606 0.417 0.5

Median 0.548 0.634 0.668 0.545 0.666 0.230 0.070 0.307 0.197 0.289 10.45 9.69 6.15 4.95 6.17 1.47 2.21 2.10 2.12 2.10 1.664 0.436 0.602 0.393 0.5

eSD 0.036 0.044 0.033 0.032 0.031 0.060 0.030 0.044 0.028 0.056 0.70 0.53 0.62 0.51 0.58 0.24 0.38 0.28 0.27 0.26 0.246 0.082 0.088 0.051 0.0

eCV 7 7 5 6 5 26 42 14 14 19 7 6 10 10 9 16 17 13 13 12 15 19 15 13 

All Lab Report 
 Round Robin XXVI Laboratory Results 

Total cis-β-Carotene Total α-Carotene Total Lycopene trans-Lycopene 

Lab

J3

FSV-BA

FSV-BD

FSV-BE

FSV-BF

FSV-BG

FSV-BH

FSV-BI

FSV-BJ

FSV-BK

FSV-BL

FSV-BN

FSV-BO

FSV-BP

FSV-BS

FSV-BT

FSV-BX

FSV-BY

FSV-BZ

FSV-CA

FSV-CB

FSV-CH

FSV-CJ

FSV-CM

FSV-CO

FSV-CP

FSV-CQ

FSV-CU

FSV-CV

FSV-CY

FSV-DC

FSV-DL

FSV-DM

FSV-DS

FSV-DY

FSV-EB

FSV-EC

FSV-EJ

168 169 170 171 172 168 169 170 171 172 168 169 170 171 172 168 169 170 171 172 168 

0.060 0.033 0.033 0.030 0.036 

0.066 0.016 0.034 0.023 0.032 

0.035 0.064 0.003 0.005 0.066 

0.029 0.034 0.031 0.033 0.027 

0.099 0.062 0.028 0.013 0.029 

0.088 0.052 0.044 0.017 0.029 

0.115 0.079 0.052 nd 0.033 

0.027 0.026 nd nd nd

0.098 0.049 0.022 0.013 0.022 

0.088 0.058 0.021 0.013 0.020 

0.072 0.048 0.018 0.012 0.018 

0.078 0.048 0.023 0.012 0.025 

0.067 0.053 0.015 nd 0.023

0.066 0.047 0.016 0.013 0.020 

0.109 0.062 0.024 0.015 0.025 

0.063 0.042 0.020 0.013 0.019 

0.125 0.071 0.028 0.016 0.029 

0.086 0.056 0.026 0.016 0.026 

na na 0.019 0.011 0.020 

0.092 0.059 0.032 0.021 0.029 

0.114 0.088 0.034 0.039 0.035 

0.440 0.450 0.300 0.230 0.270

0.472 0.522 0.342 0.246 0.304

0.398 0.392 0.264 0.334 0.221

0.338 0.276 0.192 0.156 0.183 

0.294 0.290 0.169 0.140 0.170 

0.187 0.186 0.123 0.101 0.124

0.183 0.170 0.140 0.110 0.124 

0.209 0.329 0.182 0.159 0.199 

0.202 0.200 0.139 0.132 0.155 

0.340 0.381 0.238 0.202 0.242 

0.270 0.265 0.188 0.158 0.190 

0.436 0.466 0.269 0.220 0.286 

0.362 0.384 0.230 0.196 0.222

na na 0.124 0.101 0.145 

0.215 0.249 0.183 0.175 0.199 

0.394 0.332 0.233 0.196 0.237

0.214 0.213 0.134 0.117 0.134 0.149 

0.200 

0.179 

0.108 

0.067 

0.118 

0.124 

0.130 

na 

0.111 

n 4 4 4 4 4 16 16 16 14 16 15 15 16 16 16 1 1 1 1 1 9 

Min 0.029 0.016 0.003 0.005 0.027 0.027 0.026 0.015 0.011 0.018 0.183 0.170 0.123 0.101 0.124 0.067 

Mean 0.048 0.037 0.025 0.023 0.040 0.087 0.056 0.026 0.016 0.025 0.316 0.326 0.207 0.179 0.204 0.214 0.213 0.134 0.117 0.134 0.132 

Max 0.066 0.064 0.034 0.033 0.066 0.125 0.088 0.052 0.039 0.035 0.472 0.522 0.342 0.334 0.304 0.200 

SD 0.018 0.020 0.015 0.013 0.018 0.025 0.015 0.010 0.007 0.005 0.101 0.106 0.065 0.061 0.055 0.040 

CV 38 54 59 55 44 28 26 38 44 21 32 33 31 34 27 30 

NISTa

NISTb

0.140 0.044 0.070 0.130 0.024 0.102 0.057 0.037 0.017 0.025

0.079 0.053 0.022 0.015 0.021 0.502 0.457 0.270 0.244 0.253 0.201 0.179 0.134 0.115 0.121 0.112 

Median 0.048 0.034 0.032 0.027 0.034 0.088 0.055 0.024 0.013 0.025 0.338 0.329 0.190 0.167 0.199 0.124 

eSD 0.027 0.010 0.007 0.002 0.006 0.145 0.095 0.073 0.052 0.060 0.024 

eCV 31 19 30 17 25 43 29 38 31 30 19 

All Lab Report 
 Round Robin XXVI Laboratory Results 

Total Lutein Total Zeaxanthin Total Lutein&Zeaxanthin

Lab

J4

FSV-BA

FSV-BD

FSV-BE

FSV-BF

FSV-BG

FSV-BH

FSV-BI

FSV-BJ

FSV-BK

FSV-BL

FSV-BN

FSV-BO

FSV-BP

FSV-BS

FSV-BT

FSV-BX

FSV-BY

FSV-BZ

FSV-CA

FSV-CB

FSV-CH

FSV-CJ

FSV-CM

FSV-CO

FSV-CP

FSV-CQ

FSV-CU

FSV-CV

FSV-CY

FSV-DC

FSV-DL

FSV-DM

FSV-DS

FSV-DY

FSV-EB

FSV-EC

FSV-EJ

168 169 170 171 172 168 169 170 171 172 168 169 170 171 172 

0.151 0.102 0.109 0.045 0.115 

0.157 0.137 0.112 0.046 0.111 

0.095 0.081 0.075 0.031 0.073 

0.129 0.109 0.109 0.047 0.111 

0.034 0.033 0.040 0.027 0.037 

0.038 0.036 0.043 0.023 0.043 

0.017 0.018 0.023 0.012 0.020 

0.227 0.198 0.189 0.083 0.187 

0.185 0.135 0.149 0.072 0.152 

0.186 0.159 0.149 0.071 0.151 

0.126 0.107 0.101 0.044 0.097 

0.128 0.249 0.230 0.092 0.233 

0.212 0.182 0.182 0.080 0.189 

0.341 0.263 0.169 0.079 0.157 

na na 0.158 0.071 0.162 

n 4 4 4 4 4 3 3 3 3 3 7 7 8 8 8 

Min 0.095 0.081 0.075 0.031 0.073 0.017 0.018 0.023 0.012 0.020 0.126 0.107 0.101 0.044 0.097 

Mean 0.133 0.107 0.101 0.042 0.103 0.030 0.029 0.035 0.021 0.033 0.201 0.185 0.166 0.074 0.166 

Max 0.157 0.137 0.112 0.047 0.115 0.038 0.036 0.043 0.027 0.043 0.341 0.263 0.230 0.092 0.233 

SD 0.028 0.023 0.018 0.008 0.020 0.011 0.010 0.011 0.008 0.012 0.073 0.057 0.037 0.014 0.039 

CV 21 22 17 18 19 38 33 31 38 36 36 31 23 19 24 

NISTa

NISTb 0.156 0.115 0.114 0.047 0.108 0.043 0.041 0.052 0.027 0.049 0.199 0.156 0.166 0.074 0.157 

Median 0.140 0.106 0.109 0.046 0.111 0.034 0.033 0.040 0.023 0.037 0.186 0.182 0.164 0.076 0.160 

eSD 0.061 0.070 0.024 0.007 0.027 

eCV 33 38 15 9 17 

All Lab Report 
Round Robin XXVI Laboratory Results 

Legend 

na Sample not available for analysis
 

nd Not detected (i.e., not reported or reported as '0', 'not determined', etc.)
 

italics Value calculated from reported results
 

n Number of non-NIST laboratories reporting quantitative results
 

Min Minimum non-NIST reported value.
 

Mean Average over all non-NIST reported values.
 

Max Maximum non-NIST reported value.
 

SD Standard deviation over all non-NIST values.
 

CV Coefficient of Variation (% relative standard deviation): 100*SD/Mean
 

Median Median over all non-NIST reported values 

eSD Robust estimate of SD based on the adjusted median absolute difference from the median 

(MADe) 

eCV Robust estimate of CV, 100*eSD/Median 

J5
 

All Lab Report Page 4 / 5 
% Bias Summary
 

Lab TR aT g/bT bC 

FSV-BA -2±1 3±2 -6±4 -5±3 

FSV-BD 0±1 4±6 

FSV-BE 8±5 -4±6 12±3 25±11 

FSV-BF -10±5 7±5 -4±5 42±17 

FSV-BG 5±4 6±3 8±17 

FSV-BH 0±2 0±4 -15±2 1±8 

FSV-BI -7±2 -3±1 -1±1 -6±3 

FSV-BJ -2±5 3±4 4±7 11±2 

FSV-BK 6±5 -4±4 

FSV-BL 1±6 16±5 

FSV-BN 1±2 15±2 -10±3 8±6 

FSV-BO -3±4 13±10 -8±17 

FSV-BP 7±2 5±4 -23±6 

FSV-BS 7±22 

FSV-BT -5±4 -2±3 -3±3 

FSV-BX 0±4 4±4 -2±19 

FSV-BY 2±1 -1±2 5±4 9±9 

FSV-BZ 11±4 17±8 

FSV-CA -10±2 -4±4 

FSV-CB 14±4 4±8 

FSV-CH -6±24 -10±23 -10±21 

FSV-CJ 1±3 8±9 6±6 

FSV-CM -5±7 

FSV-CO -6±1 -8±4 2±2 

FSV-CP -25±1 -9±5 

FSV-CQ 8±5 4±6 -10±40 

FSV-CU -7±4 -2±2 -6±5 

FSV-CV -1±3 6±6 28±5 27±14 

FSV-CY -3±4 -6±4 1±9 

FSV-DC -4±4 11±13 8±18 3±4 

FSV-DL 3±1 -8±1 -15±8 

FSV-DM 26±13 -11±7 26±5 

FSV-DS -2±3 -9±2 -4±4 

FSV-DY -8±16 -16±13 

FSV-EB 1±6 1±6 0±18 

FSV-EC 2±4 -2±4 -26±5 

FSV-EJ 3±3 -1±21 14±15 0±10 

NISTa 2±5 0±4 -6±8 7±10 

NISTb 19±7 -13±4 -12±4 0±4 

Label Definition 

Lab Participant code 

TR Total Retinol 

aT a-Tocopherol 

g/bT g/b-Tocopherol 

bC Total b-Carotene 

% Bias (Mean ± SD) of individual serum biases 

Mean Average of (xi

-Mediani)/Mediani 

SD Standard deviation of (xi

-Mediani)/Mediani 

xi Result for analyte in serumi 

Mediani Median of non-NIST results in serumi 

The original analysis listed % Bias for each result for 

each serum calculated relative to the "Trimmed Core 

Lab Average" of that analyte in the serum. The 

summary values reported here are the (arithmetic mean 

± standard deviation) of each laboratory's reported 

results for the analyte estimated relative to each 

serum's median value. 

J6
 
 

Appendix K. Shipping Package Inserts for RR03 

The following two items were included in each package shipped to a RR03 participant: 

• Cover letter 

• Report of Analysis datasheet 

These items were attached to the shipping box. 

K1
 
 

 

 

 

 

 

 

 

 

 

U N I TE D ST A T ES D EP A R TM E N T O F C O M M ER C E 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-0001 

August 17, 1992 

Dr. Margolis sent individual letters to invited study participants. The “~1” and “~2” 1~ 

were mail-merge commands for inserting a participant’s name and address. This 

page was prepared from a working draft. 2~ 

Thank you for agreeing to measure the ascorbic acid in the accompanying samples. The samples 

which are in sealed ampoules were prepared by adding equal volumes of spiked human serum to 

10% metaphosphoric acid (MPA). All samples have been stored at -70 °C and should be kept at 

this temperature. I have checked them for stability and the ascorbic acid appears sufficiently 

stable. 

You should find two ampoules in the shipping container. Each ampoule should be analyzed in 

duplicate by the method(s) used in your laboratory. The samples should be defrosted by 

warming at 20 °C for not more than 10 min otherwise some oxidation of ascorbic acid may 

occur. 

A report form is attached and I would appreciate it if you would make your measurements and 

return your results to me by September 25, 1992. Your results will be kept confidential. We 

will use these results in a study to demonstrate the comparative accuracy and precision of the 

laboratories currently measuring ascorbic acid. However, values will not be assigned to 

individual labs. If you wish to Telefax your results to me, the number is (301) 926-8671. 

Thank you for your assistance. 

Sincerely, 

Sam A. Margolis, Ph. D. 

Research Chemist 

Organic Analytical Research Division 

Center for Analytical Chemisty 

K2
 
 

 

 

 

 

 

 

 

 

 

 

 

REPORT OF ANALYSIS 

Name: 

Address: 

Telephone Number: 

FAX Number: 

METHOD of ANALYSIS: 

DATE of ANALYSIS:: 

SERUM 103, VIAL# 

REPLICATE 1 

REPLICATE 2 

RESULTS (μg/mL) 

________ μg/mL 

________ μg/mL 

SERUM 103, VIAL# 

REPLICATE 1 

REPLICATE 2 

________ μg/mL 

________ μg/mL 

K3
 
 

 

 

 

 

 

Appendix L. Final Report for RR03 

There is no extant version of a final report as sent to the RR03 participants. The 

following discussion and table have been extracted from a NIST-internal Report of 

Analysis that Dr. Margolis prepared in late 1993. 

The round robin data are summarized in Table 1. ... The results of the ... six 

participants [who received unthawed samples and who returned results] show a 

wide degree of variation even though the mean is relatively close to that measured 

by NIST. The LC measurements of laboratories 1 and 4 are similar to our value 

for [ascorbic acid (AA)] and probably reflect the fact that these methods are not 

measuring the [dehydoascorbic acid (DHAA)] that is present. The results of 

laboratory 6 are approximately 10% higher than those of NIST. These are 

consistent with earlier results from this laboratory using the dinitrophenylhydarzine (DNPH) method. The values reported by the other three laboratories 

probably reflect the variation in the accuracy of the various methods. The SD of 

the round robin study is approximately 13 times that of NIST and suggests that 

the data must be differentiated with respect to AA and AA + DHAA also with 

respect to the type of method used for analysis. 

Table 1. Results of the Round Robin Measurement of Ascorbic acid in Human Serum 

AA (mmol/L) 

Laboratory Method Replicate #1 Replicate #2 

1 LC-EC 54.4 54.6 

56.7 56.8 

2 LC-EC 70.4 68.1 

42.0 44.3 

3 DNPH 42.6 45.3 

65.3 63.0 

4 LC-EC 48.8 48.6 

53.4 52.2 

5 LC-EC 61.8 

61.2 

6 DNPH 72.7 72.1 

72.7 73.3 

Lab Mean ± SD 58.2 ± 10.6 (n=22) 

NIST Mean ± SD LC-EC AA 50.4 ± 3.2 (n=5) 

AA+DHAA 64.8 ± 0.8 (n=5) 

The “All Lab Report” in Appendix M provides more extensive statistical summaries. 

L1
 
Appendix M. Updated “All-Lab Report” for VC-RR03 

The following page is the updated “All-Lab Report” for RR03. 

M1
 
Vitamin C Round Robin 3
 

Lab Date Analyte Method 

VC-MB 24/02/93 HPLC-EC 

VC-MC 17/09/92 HPLC-EC 

VC-NC 25/09/92 TAA 24DNPH 

VC-NN 26/09/92 24DNPH 

VC-NR 25/09/92 AA HPLC-EC 

VC-NS 21/08/92 HPLC-EC 

NIST AA HPLC-EC 

NIST TAA HPLC-EC 

103, [AA or TAA] mmol/mL 

Mean Sdup Srep Shet Stot 

61.5 0.4 0.4 

55.6 1.6 0.1 1.6 1.6 

72.7 0.4 0.4 0.3 0.5 

54.0 14.3 1.8 14.2 14.3 

56.2 18.5 1.6 18.4 18.5 

50.2 3.6 1.3 3.5 3.7 

50.4 3.2 

64.8 0.8 

Lab 

Date 

Analyte 

Method 

Mean 

Sdup 

Srep 

Shet 

Stot 

N 

Min 

Median 

Max 

eSD 

eCV 

Revised "All Lab Report" 

N 6 

Min 50.2 0.4 0.1 0.3 0.4 

Median 55.9 2.6 1.3 3.5 2.6 

Max 72.7 18.5 1.8 18.4 18.5 

eSD 5.5 

eCV 10 

Legend 

Laboratory Code 

Date that the results were received at NIST 

Analyte specified by the laboratory 

Type of assay 

24DNPH 2,4-Dinitrophenylhydrazine
 

HPLC-EC Liquid chromatography with electrochemical detection
 

Mean of duplicate means
 

Standard deviation of duplicate means
 

Pooled standard deviation of replicates
 

Estimated sample heterogeneity,
 

Estimated standard deviation of the mean,
 

where n is the number of vials evaluated and is typically 2.
 

The number of participants 

Minimum value in the column 

Median value in the column 

Maximum value in the column 

Adjusted median absolute deviation from the median (MADe) 

Estimated coefficient of variation, 100*eSD/Median 

M2 1 / 1