NISTIR 7880-31 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1993 

Comparability Studies 

Results for Round Robins XXVII, XXVIII, and XXIX 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 4 Ascorbic Acid in Human Serum 

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.7880-31 

 

 

 

 

 

 

NISTIR 7880-31 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1993 

Comparability Studies 

Results for Round Robins XXVII, XXVIII, and XXIX 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 4 Ascorbic Acid in Human Serum 

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.7880-31 

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 1993 MMQAP measurement comparability improvement studies: 1) Round 

Robin XXVII Fat-Soluble Vitamins and Carotenoids in Human Serum, 2) Round Robin XXVIII FatSoluble Vitamins and Carotenoids in Human Serum, 3) Round Robin XXIX Fat-Soluble Vitamins 

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

materials for Round Robin XXVII were shipped to participants in January 1993; participants were 

requested to provide their measurement results by March 19, 1993. The materials for Round Robin 

XXVIII were shipped to participants in April 1993; participants were requested to provide their 

measurement results by June 14, 1993. The materials for Round Robin XXIX were shipped to 

participants in July 1993; participants were requested to provide their measurement results by 

August 30, 1993. The sample materials for Round Robin 4 were distributed in August 1993 with 

results due by September 15, 1993. 

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 XXVII: Fat-Soluble Vitamins and Carotenoids in Human Serum ....................... 1
 

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

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

Round Robin 4: Vitamin C in Human Serum................................................................................. 3
 

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

Appendix A. Shipping Package Inserts for RR27........................................................................ A1
 

Appendix B. Final Report for RR27 ..............................................................................................B1
 

Appendix C. “Individualized Report” for RR27 ..........................................................................C1
 

Appendix D. Revised “All-Lab Report” for RR27 ...................................................................... D1
 

Appendix E. Shipping Package Inserts for RR28 ......................................................................... E1
 

Appendix F. Final Report for RR28............................................................................................... F1
 

Appendix G. “Individualized Report” for RR28 ......................................................................... G1
 

Appendix H. Revised “All-Lab Report” for RR28 ....................................................................... H1
 

Appendix I. Shipping Package Inserts for RR29 ........................................................................... I1
 

Appendix J. Final Report for RR29 ................................................................................................ J1
 

Appendix K. “Individualized Report” for RR29 ......................................................................... K1
 

Appendix L. Revised “All-Lab Report” for RR29........................................................................ L1
 

Appendix M. Shipping Package Inserts for RR04 ....................................................................... M1
 

Appendix N. Final Report for RR04 ............................................................................................. N1
 

Appendix O. Revised “All-Lab Report” for RR04 ...................................................................... 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 XXVII: Fat-Soluble Vitamins and Carotenoids in Human Serum 

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

XXVII comparability study (hereafter referred to as RR27) received five 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 1993. 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 RR27 is reproduced as Appendix B. This report 

included: 

• Our analysis of the participants’ results. 

• Tabular presentations of all participant results 

• Graphical presentations of “Interlaboratory Precision vs Time” 

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 RR27 in a more accessible format. 

1
 
 

 

 

 

 

 

 

 

 

 

 

 

 

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

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

XXVIII comparability study (hereafter referred to as RR28) received five 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 April 1993. 

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 RR28 is reproduced as Appendix F. This report 

included: 

• Our analysis of the participants’ results. 

• Tabular presentations of all participant results 

• Graphical presentations of “Interlaboratory Precision vs Time” 

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

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

Appendix H lists all of the measurement results reported for RR28 in a more accessible format. 

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

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

XXIX comparability study (hereafter referred to as RR29) 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 July 1993. 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. 

A preliminary report for RR29 was mailed to all participants shortly before the Micronutrients QA 

Workshop held on October 1993. The “Summary of 1993 Round Robin Activities” was mailed to 

every participant in the 1993 program in November 1993. This Summary included lists of all the 

Fat-Soluble Vitamin MMQAP results for RR27 and RR28 as well as RR29. The cover letter of the 

preliminary report and the RR29-related components of the Summary are reproduced as Appendix J. 

Each participant also received an “Individualized Report” that graphs their RR29 results for selected 

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

Appendix L lists all of the measurement results reported for RR29 in a more accessible format. 

2
 
 

 

 

 

 

 

 

Round Robin 4: Vitamin C in Human Serum 

Participants in the MMQAP Vitamin C in Human Serum Round Robin 4 comparability study 

(hereafter referred to as RR04) received six frozen serum test samples, two ampoules of each of 

three different materials. These samples were shipped on dry ice to participants in August 1993. 

The available communication materials included in the sample shipment are described in Appendix 

M. 

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. 

The final report delivered to all participants in RR04 consists of a cover letter and a series of Tables 

and Figures that summarize the results of the study. This report is reproduced as Appendix N. 

While not distributed to the participants in RR04, Appendix O is 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 RR04. 

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 RR27 

Two slightly different sets of samples were distributed in RR27. All participants received two 

vials each of Sera 173 to 174. In addition, “Core labs” – those who had participated in at least 

the 1991 and 1992 Round Robin studies – received one vial of Serum 177. The Core and nonCore participants received different letters and datasheets. 

The following two items were included in each package shipped to an RR27 participant: 

•	 Cover letter. The original letters have been lost. The attached version has been 

reconstructed from a letter sent to a participant who enrolled in the 1993 program after 

RR27 had been shipped. This version represents what was sent to the Core labs; the 

version sent to non-Core labs would excluded the information on Serum 177. 

•	 Datasheet. As with the cover letter, the attached version is what was sent to the Core 

labs. The version sent to the non-Core labs deleted the spaces provided for Serum 177 

results and the comment that only one vial of Serum 177 was available per participant. 

These items were attached to the shipping box. 

A1
 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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 

January 11, 1993 

Dear Colleague: 

The 1993 NIST/NCI Fat-Soluble Vitamins Quality Assurance Program w i l l consist of 

three Round Robin exercises. The core analytes in the program will be: retinol, retinyl 

palmitate, α-tocopherol, γ-tocopherol, and total β-carotene. Data will also be collected 

and analyzed for α-carotene, trans-β-carotene, β-cryptoxanthin, lutein, total lycopene, 

trans-lycopene, and zeaxanthin. One of the three studies is designed to focus primarily on 

problems associated with selected carotenoid compounds. 

Enclosed is the set of samples for the first 1993 Round Robin exercise (Round Robin 

XXVII). You will find duplicate vials of four lyophilized sera samples (Sera 173 to 

176) and one vial of Serum 177 for analysis along with a form for reporting your results. 

When reporting your results, please submit one value for each analyte for a given 

serum sample. 

Samples should be reconstituted with 1.00 mL of HPLC Grade water or equivalent. We 

recommend that dissolution be facilitated with 3 to 5 minutes agitation in an ultrasonic 

bath or at least 30 min at room temperature with intermittent swirling. (CAUTION: 

Vigorous shaking will cause foaming and possibly interfere with accurate measurement. 

The rubber stopper contains phthalate esters which will leach into the sample upon 

intermittent contact of the liquid sample with the stopper. These esters absorb strongly 

in the UV region and elute very near retinol in most HPLC systems creating analytical 

problems.) Pipette a known volume of serum from the vial for analysis since the final 

volume of the reconstituted sample is greater than 1.0 mL. For consistency, we h av e 

requested that laboratories use the following absorptivities (E1% cm) in ethanol: retinol, 

1850 at 325 nm; retinyl palmitate, 975 at 325 nm; α-tocopherol, 75.8 at 292 nm; 

γ-tocopherol, 91.4 at 298 run; α-carotene, 2800 at 444 nm; β-carotene, 2560 at 450 nm; 

lycopene, 3450 at 472 nm. We understand that there is some discrepancy in the reported 

absorptivities and studies are currently underway to identify certified values in ethanol and 

hexane. 

Results for Round Robin XXVII are due to NIST by March 19, 1993. Results may be 

mailed or FAXed to: 

Ms. Nancy T. Miles 

NIST 

Bldg. 222, Rm. B158 

Ga1tnersburg, MD 20899 USA 

FAX: (301) 926-8671 

A2
 
 

Analytical and technical queries should be directed to me at the same address or via 

telephone at (301) 975-3208. 

This year’s workshop is being planned for late September. You will be informed of the 

actual date and meeting place. 

Sincerely, 

Willie E. May, Ph.D. 

Chief 

Organic Analytical Research Division 

Chemical Science and Technology Laboratory 

A3
 
ROUND ROBIN XXVII RESULTS FROM LABORATORY # _________ 

DATE OF ANALYSIS ___________ 

RESULTS IN ug/mL 

SAMPLE NUMBER ANALYTE RESULT 

SERUM 173 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 174 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 175 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 176 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 177 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

OPTIONAL ANALYTES: SUPPLY ONE RESULT IF AVAILABLE 

SERUM # 173 174 175 176 177 

TRANS-BETA CAROTENE 

ALPHA-CAROTENE 

RETINYL PALMITATE 

GAMMA-TOCOPHEROL 

LYCOPENE (TOTAL) 

9-CIS-BETA CAROTENE 

13-CIS-BETA-CAROTENE 

LUTEIN 

ZEAXANTHIN 

BETA-CRYPTOXANTHIN 

DIRECTIONS: Reconstitute with 1.0 mL distilled water. 

COMMENT: Only 1 vial of Serum 177 is available per lab. 

FAX RESULTS TO 301/926-8671 

A4
 
 

 

 

Appendix B. Final Report for RR27 

The following eleven pages are the final report for RR27 as provided to all participants. 

This report consists of: 

•	 A cover letter and discussion. 

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

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

•	 Tables 5 to 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, trans-lycopene, 

total cis-β-carotene, trans-α-carotene, and δ-tocopherol. 

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

retinol, α-tocopherol, and total 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 RR27 results where the original codes have been altered to ensure 

confidentiality. Appendix D also provides more relevant summary statistics. 

B1
 
April 28, 1993 

Dear Colleague: 

N~ UNITEC STATES CEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899 

This report describes both overall-group and your laboratory's performance in Round Robin 

XXVII. Specifically, your package contains for retinol, a-tocopherol, and /3-carotene, 

respectively: tabular presentations of all data submitted for Round Robin XXVII; a Blind Control 

Chart representing a summary of your laboratory's data vs the assigned values for the past six 

years; and a graphical presentation of data from your laboratory's analysis of blind duplicate 

samples. Tabular data only is provided for 11-tocopherol, o-tocopherol, all-trans /3-carotene, 

trans a-carotene, a-carotene, retinyl palmitate, total and trans-lycopene, lutein, zeaxanthin, /3-

cryptoxanthin, and total cis-/3-carotene. 

As indicated in the tables, each of the samples in Round Robin XXVII (Serum 173-177) had 

been distributed as part of previous round robins. For example, Serum 173, the mid-level of 

SRM 968a, was previously distributed as Sera 149 and 159. Serum 177, the high-level of SRM 

968a, was previously distributed as Sera 150 and 161. As part of a study to monitor the stability 

of the fat-soluble vitamins in SRM 968a, Serum 177 was distributed to only the Core labs 

(program participants for more than two years) in this round robin exercise. 

Table 1 provides a summary of the data submitted for retinol in Round Robin XXVII. Thirtyeight labs submitted data: 27 Core labs and 11 New labs, 8 with one- to two-year participation 

and 3 participating in our round-robin study for the first time. As shown in Table 1, the mean 

relative standard deviation (RSD) for All and Core laboratory retinol measurements approached 

13%. The mean RSD for the trimmed Core labs, however, was about 6% for retinol. The Core 

labs mean RSD for retinol over the past two years has ranged from 8. 7 - 12. 7 % . The mean RSD 

for the New labs with one- to two-year participation ranged from 9. 9 - 18 % . The mean RSD 

for those labs participating for the first time was about 3 % . The overall values obtained for 

retinol in this round robin were comparable to those obtained in the previous round robin 

studies. 

Table 2 provides a summary of data submitted for the determination of a-tocopherol in Round 

Robin XXVII. Thirty-four laboratories submitted data: 25 Core labs; 8 one- to two-year 

participants; and 1 first-time participant. The mean RSD for Core labs was about 9%, while 

the mean RSD for New labs with one- to two-year participation ranged from about 12.5 - 18 % . 

The overall RSD for the Core labs has remained in the 9 - 11 % range over the past two years. 

Again, there was no significant change in values for a-tocopherol in this study and the previous 

round robin studies. 

Table 3 provides a summary of data for total /3-carotene. Thirty-three laboratories submitted 

data: 24 Core labs; 7 one- to two-year participants; and 2 first-time participants. As in recent 

studies, the overall quality of the /3-carotene data is slightly poorer than for retinol and atocopherol. The mean RSD for All labs was about 34 % , while the mean RSD for the Core labs 

B2
 
Page 2 

April 28, 1993 

was about 26%. In the last round-robin exercise, the mean RSD for the Core labs was 16% and 

was > 20 3 over the past two years. The mean RSD for the trimmed Core labs in this study 

was about 14 % . There is no obvious correlation between RSD and concentration. 

Tables 4-16 provide summaries of RRXXVII data submitted for other fat-soluble vitamins and 

carotenoid compounds. Data submitted for y-tocopherol again appears to show improvement 

with the RSD for the trimmed lab average being around 7. 7 3. Except for trans P-carotene and 

lycopene, the concentrations of the remaining analytes appear to be too low for a fair assessment 

of either individual or interlaboratory measurement capabilities. 

Data for your use in evaluating your laboratory's individual performance in RRXXVII is 

provided on the right side of Tables 1-4. The Core labs trimmed values were used as the 

assigned values. By convention, 0-5 % bias from the assigned value represents EXCEPTIONAL 

performance, 6-10% ACCEPTABLE performance, 11-20% MARGINAL performance and 

>20% POOR performance relative to the current state of the art for these measurements. If 

you have concerns regarding your performance or are a lab whose performance would be rated 

"U" based on the convention stated above, we suggest that you obtain a unit of SRM 968a and 

analyze all three levels. If, with minor method modifications, your measured values do not 

agree with the certified values, feel free to contact us for consultation. SRM 968a can be 

obtained through the NIST Standard Reference Materials Program (3011975-6776). 

Round Robin XXVIII samples were shipped during the week of April 26. If you have not 

received them, please call Nancy Miles at 3011975-3108. Results will be due by June 14 and 

we expect to provide you feedback concerning your performance by July 26. Results from all 

three 1993 lnterlaboratory Studies will be discussed at our Annual QA Workshop in the fall. 

As some of you are perhaps aware, Dr. Neal Craft has resigned his position at NIST. Calls 

concerning various aspects of the round robin studies should be directed to me at 3011975-3108 

or Ms. Jeanice Brown Thomas at 3011975-3120. 

Sincerely, 

Willie E. May, Ph.D. 

Chief 

Organic Analytical Research Division 

Chemical Science and Technology Laboratory 

Enclosures 

B3
 
Table 1. Round Robin XXVII 

Retinol Results 

Lab# 

NIST 1 

NIST 3 

All Labs 

AVG (38) 

SD 

RSD 

Core Labs 

AVG 

SD 

RSD 

Serum# 

173 

a.493 

a.449 

a.SS2 

•a.S83 

a.499 

a.46S 

a.S2S 

a .491 

•a.381 

a.498 

a.S24 

a.sa6 

a.sos 

a.4S2 

o.sao 

0.S21 

O.S40 

0.49S 

a.S33 

a.491 

0.482 

a .508 

O.Sl4 

•a. 3S2 

*O.S96 

a.497 

*0.432 

a.468 

a. 671 

O.SS7 

0.463 

0.28S 

a.sa4 

a.S29 

0.48a 

a.s8a 

0.448 

O.Sa3 

0.480 

a.sos 

0.880 

a.sa2 

o.soa 

0.517 

0.482 

o.sa3 

O.OS6 

11.1 

a .496 

O.OS2 

10.S 

(a) New Labs 

AVG 

SD 

RSD 

(b) New Labs 

AVG 

SD 

RSD 

(c) New Labs 

AVG 

SD 

RSD 

0.S49 

o.a90 

16.4 

a.5a9 

O.OS8 

11.3 

a.496 

o.a14 

2.8 

Serum# 

174 

O.S27 

*0.4SO 

O.S38 

*0.644 

O.S85 

a.S08 

a.57a 

a.556 

a.480 

a.5S4 

0.572 

a.545 

a.527 

a.S89 

•a.32a 

a.s3a 

a.S97 

0.S28 

a.S76 

a.soo 

a.509 

a.S38 

a.538 

•a.383 

*0.673 

a.S23 

•a.4S4 

a.sl3 

0.756 

0.585 

a .467 

a. 298 

0. 577 

0.624 

0.5SO 

0.561 

0.491 

0.532 

0.5ao 

0.530 

0.920 

O.S54 

0.54a 

0.542 

0.502 

0.539 

0.074 

13.8 

O.S30 

a.072 

13.5 

0. 596 

a.119 

20.0 

a.SS7 

a.aS4 

9.8 

a.S21 

a.al8 

3.4 

Serum# 

175 

0. 4a5 

0.366 

0.377 

a.39a 

0.368 

0.367 

0.431 

a .418 

0.3S5 

0.4a5 

a.414 

0. 397 

0 .422 

0. 386 

0.38a 

0.414 

*O.S62 

0.386 

a.419 

0.383 

0.375 

a.44a 

0 .396 

*0.322 

*0.473 

0.407 

0.346 

0. 382 

0.508 

0.449 

0.347 

0.245 

0.429 

0.467 

0 .410 

0.401 

0.366 

0.403 

0.390 

0 .401 

0.710 

0.394 

0 .420 

0.407 

0.372 

0.405 

0.045 

11.1 

0 .400 

0.045 

11.2 

Serum# 

176 

0.536 

0.503 

*0.691 

0. 613 

0 .Sl3 

O.Sl7 

0.597 

0.542 

0.476 

0.536 

0.561 

O.S28 

O.S76 

O.S31 

O.S40 

0.580 

a.588 

O.S38 

O.S47 

0.SOl 

O.S06 

O.SS2 

O.S41 

*.0398 

*0.676 

O.Sl9 

*0.4S6 

0.S37 

0.737 

0.581 

0.481 

0. 34S 

0.513 

0. 572 

0 .490 

0.534 

0.478 

O.S41 

0. S30 

0.S84 

0.860 

0.537 

0.610 

O.S62 

O.S47 

O.S4S 

0.063 

11.S 

O.S43 

0.060 

11. 0 

2 yr participation. 

a.433 

o.a67 

lS.4 

O.S78 

a.114 

19.7 

Serum# 

177 

0.644 

*0.538 

0.673 

0.750 

0.624 

0.609 

0. 704 

0.653 

*0.496 

0. 712 

0.694 

0.621 

0.67S 

0.630 

0.640 

0. 718 

a.69S 

0.661 

a.6S2 

0. 611 

0.692 

0. 72a 

*l. 119 

0.74S 

a.643 

•a.S70 

0.632 

0.643 

a.673 

a.109 

16.2 

a.673 

a.109 

16 .2 

1-2 yr participation. 

a.411 

a.042 

10.2 

O.Sl9 

o.a43 

8.3 

First time participation. 

0.398 

a.oa7 

l. 8 

a.ss2 

a.a29 

S.2 

% Bias from Trimmed Core Lab Average. 

Lab# 

Serum# 

173 

-1. 7 

-la.s 

la.a 

16.2 

-a.s 

-7.4 

4.6 

-2.1 

-24.1 

-a.7 

4.4 

a.8 

a.6 

-9.9 

-a.3 

3.8 

7.6 

-1. 3 

6.1 

-2.1 

-3.9 

1.2 

2.4 

-29.8 

18.8 

-a.9 

-13.9 

-6.7 

33.7 

11.a 

-7.7 

-43.2 

a.4 

5.4 

-4.3 

15.6 

-la.6 

a.2 

-4.3 

a.6 

75.4 

o.a 

-a.3 

Core Labs Trimmed 

AVG 

SD 

RSD 

O.S02 

a.a26 

S.l 

Serum# 

174 

-2.8 

-17.a 

-a.8 

18.7 

7.9 

-6.4 

S.l 

2.S 

-11. s 

2.1 

s.s 

a.s 

-2.8 

8.6 

-41. a 

-2.3 

10.1 

-2.6 

6.2 

-7.8 

-6.l 

-a. 8 

-a.8 

-29.4 

24.1 

-3.6 

-16.3 

-5.4 

39. 4 

7.9 

-13.9 

-45.1 

6.4 

15.l 

1.4 

3.4 

-9.4 

-1. 9 

-7.8 

-2.3 

69.6 

2.1 

-0 .4 

a.542 

a.a31 

S.7 

Serum# 

175 

2.9 

-7.a 

-4.2 

-a.9 

-6.S 

-6.8 

9.S 

6.2 

-9.8 

2.9 

S.2 

a.9 

7.2 

-1. 9 

-3.5 

S.3 

42.8 

-1. 9 

6.4 

-2.7 

-4.7 

11. 7 

a.6 

-18.2 

2a.2 

3.4 

-12.l 

-3.0 

29.1 

14.1 

-11.8 

-37.8 

9.0 

18.6 

4.2 

1.9 

-6.9 

2.4 

-a.9 

1. 9 

8a.4 

a.l 

6.7 

0.394 

a.a25 

6.2 

Serum# 

176 

-a.9 

-7.0 

27.7 

13.3 

-5.2 

-4.4 

la.4 

a.2 

-12.0 

-a.9 

3.7 

-2.4 

6.5 

-1. 8 

-a.2 

7.3 

8.7 

-a.5 

1.1 

-7.4 

-6.S 

2.a 

a.a 

-26.4 

2S.O 

-4 .1 

-lS.7 

-a.7 

36.3 

7.4 

-11.1 

-36.2 

-S.2 

S.7 

-9 .4 

-1. 3 

-11. 6 

o.a 

-2.a 

8.a 

S9.a 

-a.7 

12.8 

0 .S41 

a.a33 

6.2 

Serum# 

177 

-4.a 

-19.8 

0.3 

11. 7 

-7.a 

-9. 3 

4.9 

-2.7 

-26 .1 

6.1 

3.4 

-7.S 

0.6 

-6.l 

-4.6 

7.0 

3.6 

-1.5 

-2.9 

-9.0 

3.1 

7.3 

66.7 

11.0 

-4.2 

-15.l 

a.671 

a.042 

6.3 

PREVIOUS S/91 149 S/91 15a 

VALUE a.489 8/91 1S5 8/91 156 8/92 171 0.6S9 

8/91 159 a.S36 a.4a5 a.S38 1/92 161 

0.Sa6 0.673 

Value removed for Core Lab Trimmed Average. 

L Late results not included in statistical analysis. 

B4
 
Table 2. Round Robin XXVII 

Alpha-Tocopherol 

Lab# 

Serum# 

173 

NIST 1 

NIST 3 

All Labs 

AVG (34) 

SD 

RSD 

Core Labs 

AVG 

SD 

RSD 

(a) New Labs 

AVG 

SD 

RSD 

(b) New Labs 

AVG 

SD 

RSD 

(c) New Labs 

Value 

10.40 

9. 71 

10.65 

10.14 

*9 .12 

10.26 

11.70 

11.12 

10.67 

11.42 

10.34 

11. 04 

10.10 

9.58 

10.50 

11.40 

11.35 

11.15 

10.05 

10.90 

10.11 

11.10 

11.30 

10.95 

*8.70 

7.84 

8.41 

11. 96 

11.18 

8.73 

8.24 

13.01 

10.32 

11. 63 

9.54 

10.00 

15.90 

10. 85 

10.80 

10.76 

10.53 

10.53 

1. 02 

9.7 

10.55 

0.75 

7.1 

9.95 

1.90 

19.1 

11.13 

1.52 

13.7 

10.00 

Serum# 

174 

7.35 

*6.52 

7.24 

7.00 

7.38 

7.10 

7.98 

7.84 

7.61 

7.90 

7.45 

7.63 

*8.99 

*6.30 

*4.53 

7.30 

7.61 

7. 71 

7.04 

7. 92 

7.33 

7.67 

8.14 

7.76 

*6.46 

4.70 

5.83 

7.97 

8.09 

6.15 

6.05 

9.66 

7.65 

8.39 

6.70 

6.50 

10.70 

7. 80 

7.60 

7.48 

7. 96 

7.37 

0.93 

12.6 

7.35 

0.82 

11.1 

6.98 

1.21 

17.3 

8.10 

1.25 

15.4 

6.50 

Serum# 

175 

10.08 

9.31 

9.50 

9.13 

*8.69 

9.57 

10.40 

10.71 

9.50 

11. 00 

10.01 

10.24 

11. 00 

10.80 

10.57 

10.30 

10.54 

10.76 

9.00 

9.77 

9.56 

10.15 

10.10 

10.73 

*8.12 

8 .40 

7.02 

ll.42 

10.03 

8.58 

8.95 

11. 30 

9.06 

11. 25 

8.93 

10.20 

16.70 

10.50 

10.40 

9.77 

10.28 

9.93 

0.97 

9.7 

9.98 

0.75 

7.6 

Serum# 

176 

4.93 

4.61 

5.70 

4.73 

3.95 

4.53 

*6.10 

5.13 

4.84 

5.20 

5.13 

5.15 

5.55 

3.69 

4.93 

5.00 

5.14 

4.94 

4.49 

5.28 

5.02 

4.91 

3.64 

4.36 

3.64 

3.58 

4.74 

5.62 

6.17 

4.25 

4 .31 

5.00 

4.78 

5.43 

4.50 

4.50 

7.20 

5.20 

4.80 

4.72 

5.03 

4.87 

0.61 

12.6 

4.82 

0.62 

12.8 

2 yr participation. 

9.36 

1. 86 

19.8 

5.21 

0.84 

16 .2 

Serum# 

177 

16.01 

*13 .16 

15.73 

15.67 

14.36 

15.20 

17.00 

15.53 

15.11 

17.20 

16.21 

17.15 

17.00 

*19.16 

15.60 

16.30 

16.57 

16.19 

13. 87 

15.82 

14.43 

14 .50 

16.23 

13.72 

7.20 

15.78 

15.80 

15.74 

1.33 

8.5 

15.74 

1.33 

8.5 

1-2 yr participation. 

10.13 

1. 32 

13. 0 

4.93 

0.39 

7.9 

First time participation. 

10.20 4.50 

% Bias from Trimmed Core Lab Average. 

Lab# 

Serum# 

173 

-2. 7 

-9.2 

-0.4 

-5.2 

-14.7 

-4 .1 

9.4 

4.0 

-0.2 

6.8 

-3.3 

3.2 

-5.5 

-10.4 

-1. 8 

6.6 

6.1 

4.2 

-6.0 

1. 9 

-5.5 

3.8 

5.7 

2 .4 

-18.6 

-26.7 

-21.4 

11. 8 

4.5 

-18.4 

-23.0 

21. 7 

-3.5 

8.8 

-10.8 

-6.5 

48.7 

1.5 

1. 0 

Core Labs Trimmed 

AVG 

SD 

RSD 

10.69 

0.59 

5.5 

Serum# 

174 

-2. 6 

-13.6 

-4.1 

-7.3 

-2.2 

-5.9 

5.7 

3.9 

0.8 

4.7 

-1. 3 

1.1 

19.1 

-16.5 

-40.0 

-3.3 

0.8 

2.1 

-6.8 

4.9 

-2. 9 

1. 7 

7.8 

2.8 

-14.4 

-37.7 

-22.8 

5.6 

7.1 

-18.5 

-19.8 

28.0 

1.4 

11.1 

-11.2 

-13.9 

41. 8 

3.3 

0.7 

7.55 

0.33 

4.3 

Serum# 

175 

-0.4 

-8.0 

-6.l 

-9.8 

-14.l 

-5.4 

2.8 

5.8 

-6.1 

8.7 

-1. 0 

1.2 

8.7 

6.7 

4.5 

1. 8 

4.2 

6.4 

-11.1 

-3.5 

-5.6 

0.3 

-0.2 

6.0 

-19.8 

-17.0 

-30.6 

12.9 

-0.9 

-15.2 

-11.5 

11. 7 

-10.5 

11.2 

-11. 8 

0.8 

65.0 

3.8 

2.8 

10.12 

0.61 

6.0 

Serum# 

176 

3.3 

-3.3 

19.5 

-0.8 

-17.2 

-5.0 

27.9 

7.6 

1.5 

9.0 

7.5 

8.0 

16.4 

-22.6 

3.4 

4.8 

7.8 

3.6 

-5.9 

10.7 

5.1 

2.9 

-23.7 

-8.6 

-23.8 

-24.9 

-0.6 

17.8 

29.4 

-10.9 

-9.7 

4. 8 

0.2 

13. 7 

-5.7 

-5.7 

51. 0 

9.0 

0.6 

4.77 

0.57 

11. 9 

Serum# 

177 

2.0 

-16.2 

0.2 

-0 .2 

-8 .5 

-3.2 

8.3 

-1.1 

-3.8 

9.6 

3.2 

9.2 

8.3 

22.0 

-0.6 

3.8 

5.5 

3.1 

-11. 7 

0.7 

-8.l 

-7.6 

3.4 

-12.6 

15.70 

1.03 

6.6 

PREVIOUS 5/91 149 5/91 150 

VALUE 10.50 8/91 155 8/91 156 8/92 171 16.59 

8/91 159 7.55 10.16 5.03 1/92 161 

10.42 15.95 

Value removed for Core Lab Trimmed Average. 

B5
 
Table 3. Round Robin XXVII 

Lab# 

NIST l 

NIST 3 

All Labs 

AVG (33) 

SD 

RSD 

Core Labs 

AVG 

SD 

RSD 

Serum# 

173 

0.957 

0.853 

0.830 

*1.377 

0.965 

0.921 

0.836 

*l.130 

0.980 

0.964 

l. 020 

0. 927 

0.930 

0.946 

0.930 

0.874 

0.933 

*l.129 

0.786 

*0.695 

0.932 

0.862 

0.853 

*0.719 

0.325 

l.067 

0.890 

0.902 

0.993 

0.367 

0.840 

0.990 

0.705 

l.760 

0.907 

0.892 

0.868 

0.936 

0.223 

23.9 

0.931 

0.143 

15.4 

(a) New Labs 

AVG 

SD 

RSD 

(b) New Labs 

AVG 

SD 

RSD 

(c) New Labs 

AVG 

SD 

RSD 

.983 

. 089 

9.0 

0.726 

0.266 

36.6 

l.334 

0.603 

45.2 

Total Beta-Carotene 

Serum# 

174 

0.387 

0.332 

0.300 

0.481 

0.410 

0.355 

0.275 

0. 490 

0.369 

0.377 

0.421 

0.428 

0.386 

0.377 

0.300 

0.361 

0. 348 

0.464 

0.325 

0.296 

0.372 

0.344 

0.341 

*l.120 

0.309 

0.089 

0.231 

0.570 

0.371 

0.383 

0.145 

0.423 

0.379 

0.300 

l.330 

0.389 

0.315 

0.343 

0.416 

0.224 

53.9 

0.399 

0.164 

4l. l 

Serum# 

175 

0.968 

0.774 

0.728 

*l. 276 

0.858 

0.972 

0.722 

l. 040 

0 .874 

0.866 

0.923 

l.020 

0.820 

0.977 

0.900 

0. SU 

0.850 

0.980 

0.644 

0.640 

0.932 

0.634 

0.734 

*0.395 

0.721 

0.346 

0.999 

0.794 

0. 791 

0.926 

0.429 

0.823 

0.889 

0.627 

2 .310 

0.832 

0.693 

0.782 

0.875 

0 .311 

35.6 

0.843 

0.178 

2l.2 

Serum# 

176 

0.442 

0.361 

0.324 

0.528 

0.412 

0. 412 

*0.204 

0.480 

0.406 

0.410 

0.435 

0.504 

0.386 

0 .416 

0.470 

0.412 

0.429 

0.477 

0.350 

0.294 

0.434 

0.463 

0.335 

*O. 996 

0.316 

0.171 

0.401 

0.485 

0.340 

0.382 

0.196 

0.376 

0.424 

0.305 

l. 040 

0.422 

0.322 

0 .413 

0.435 

0.169 

38.8 

0.430 

0.141 

32.9 

2 yr participation. 

0.395 

0.170 

43.0 

0.312 

0.122 

39.2 

0.860 

0.665 

77.4 

0.906 

0.104 

ll .5 

0. 692 

0.208 

30.0 

l.571 

l.045 

66.5 

0.423 

0.055 

13 .0 

0.325 

0.099 

30.5 

0. 731 

0.437 

59.8 

Serum# 

177 

2.583 

l.823 

2.034 

2.950 

2.364 

2.390 

l. 830 

3.070 

2.418 

2.259 

2.500 

2.860 

2.286 

2.880 

2.347 

2.461 

1. 963 

l. 635 

2.530 

2.205 

1. 900 

3.190 

2.037 

l. 950 

2.220 

2.374 

0.430 

18.l 

2.374 

0.430 

18.l 

Lap# 

% Bias from Trimmed Core Lab Average. 

Serum# 

173 

5.2 

-6.2 

-8.7 

51.4 

6.l 

l.3 

-8.l 

24.3 

7.8 

6.0 

12.2 

l. 9 

2.3 

4.0 

2.3 

-3.9 

2.6 

24.2 

-13.6 

-23.6 

2.5 

-5.2 

-6.2 

-20. 9 

-64.3 

17.3 

-2.l 

-0.8 

9.2 

-59.6 

-7.6 

8.9 

-22. 5 

93.5 

-0.3 

Serum# 

174 

5.2 

-9.8 

-18.5 

30.7 

ll.4 

-3.5 

-25.3 

33.2 

0.3 

2.5 

14.4 

16.3 

4.9 

2.5 

-18.5 

-l. 9 

-5.4 

26.l 

-ll. 7 

-19.5 

l.l 

-6.5 

-7.3 

204.4 

-16.0 

-75.8 

-37.2 

54.9 

0.8 

4.l 

-60.6 

15.0 

3.0 

-18.5 

261.5 

5.7 

Serum# 

175 

l4. 7 

-8.3 

-13. 7 

5l.2 

l.6 

15.2 

-14.5 

23.2 

3.6 

2.6 

9.4 

20. 9 

-2.8 

15.8 

6.6 

-4.0 

0.7 

16.1 

-23.7 

-24.2 

10 .4 

-24. 9 

-13. 0 

-53.2 

-14.6 

-59.0 

18.4 

-5.9 

-6.3 

9.7 

-49.2 

-2.5 

5.3 

-25.7 

173.7 

-l.4 

Serum# 

176 

6.8 

-12.8 

-21. 7 

27.5 

-0.6 

-0.5 

-50.7 

15.9 

-l. 9 

-l. 0 

5.l 

21. 7 

-6.8 

0.5 

l3 .5 

-0.6 

3.6 

15.2 

-15.5 

-29.1 

4.8 

ll. 8 

-19.l 

140. 6 

-23.7 

-58.7 

-3.l 

17.l 

-17.9 

-7.7 

-52.7 

-9.2 

2.4 

-26.3 

151.2 

l. 9 

Serum# 

177 

8.8 

-23.2 

-14.3 

24.3 

-0 .4 

0.7 

-22.9 

29. 3 

l. 9 

-4.8 

5.3 

20. 5 

-3.7 

2l. 3 

-l. l 

3.7 

-17.3 

-3l.2 

6.6 

-7.l 

-20.0 

34.4 

-l4 .2 

Core Labs Trimmed 

AVG 

SD 

RSD 

0.909 

0.062 

6.8 

0.368 

0. 059 

16.l 

0.844 

0 .128 

15.2 

0.414 

0.063 

15.l 

2.374 

0.430 

18.l 

PREVIOUS 5/91 149 5/91 150 

VALUE 0.890 8/91 155 8/91 156 8/92 171 2.338 

8/91 159 0.371 0.822 0.416 1/92 161 

0. 879 2.212 

Value removed for Core Lab Trimmed Average. 

L Late results not included in statistical analysis. 

B6
 
Table 4. Round Robin XXVII 

Lab# 

NIST 1 

NIST 3 

AVG 

SD 

RSD 

Serum# 

173 

2.83 

2.55 

2.70 

2.90 

2.64 

3.20 

2.82 

2.95 

3.09 

2.94 

2.77 

2.27 

*2.18 

2.19 

3.02 

2.96 

2.77 

2.81 

0.26 

9.3 

Gamma Tocopherol 

Serum# 

174 

2.24 

2.00 

2.32 

2.40 

2.15 

2.58 

2.85 

2.22 

2.70 

2.35 

2.28 

1.76 

1. 76 

1. 77 

2.50 

2 .42 

2.23 

2.33 

0.29 

12.3 

Serum# 

175 

1. 97 

1. 78 

1. 94 

2.10 

1. 88 

2.23 

2 .11 

2.03 

2 .18 

2.06 

1. 90 

1. 69 

*1.53 

1. 33 

2 .13 

1. 94 

1. 98 

1. 99 

0.19 

9.5 

Table 5. Round Robin XXVII 

Trans-Beta-Carotene 

Lab# 

NIST 1 

NIST 3 

AVG 

SD 

RSD 

Serum# 

173 

0.895 

0.957 

0.726 

0.942 

0.862 

0.786 

0.880 

0.106 

12.0 

Serum# 

174 

0.345 

0 .396 

0.293 

0.362 

0 .312 

0.311 

0.349 

0.043 

12.3 

Serum# 

175 

0. 814 

0.877 

0.599 

0. 856 

0.659 

0.731 

0.787 

0.128 

16.2 

Serum# 

176 

2.14 

1. 97 

2.12 

2 .10 

2.01 

2.48 

2.40 

2.05 

2.32 

*3.47 

1.93 

1. 79 

1.84 

1. 75 

2.27 

2 .13 

2.27 

2.24 

0.41 

18.5 

Serum# 

176 

0.376 

0.403 

0. 313 

0.404 

0.288 

0.374 

0.374 

0. 043 

11.4 

Serum# 

177 

3.90 

*3.12 

3.85 

4.00 

3.65 

*4.55 

4.13 

3.79 

3.96 

3.75 

3.85 

3.87 

3.87 

0.36 

9.4 

Serum# 

177 

2.055 

2.362 

1.836 

1.760 

2. 000 

2.084 

0.264 

12.7 

% Bias from Trimmed Core Lab Average. 

Lab# 

Serum# 

173 

-1. 3 

-11.1 

-5.8 

1.2 

-7.9 

11.6 

-1. 6 

2.8 

7.8 

2.5 

-3.4 

-20. 8 

-24.0 

-23.6 

5.2 

Trimmed Lab Average 

AVG 

SD 

RSD 

2.87 

0.19 

6.6 

Serum# 

174 

-4.0 

-14. 3 

-0.6 

2.8 

-8.1 

10.5 

22.1 

-4.9 

15.7 

0.7 

-2.3 

-24.6 

-24.4 

-24.2 

7.0 

2.33 

0.29 

12.3 

Serum# 

175 

-2.8 

-12.l 

-4.2 

3.7 

-7.4 

10.1 

4.2 

0.4 

7.6 

1. 7 

-6.2 

-16.6 

-24.5 

-34.3 

5.1 

2. 03 

0 .13 

6.7 

Table 6. Round Robin XXVII 

Alpha-Carotene 

Lab# 

NIST 

AVG 

SD 

RSD 

Serum# 

173 

0.047 

0.048 

0.049 

0.065 

0.050 

0.054 

0.050 

0.062 

0.042 

0.079 

0.036 

0.053 

0.040 

0.038 

0.089 

0.059 

0.055 

0.049 

0.023 

0.048 

0.068 

0.052 

0.015 

28.2 

Serum# 

174 

0.026 

0.021 

0.035 

0.022 

0.020 

0.022 

0.017 

0.031 

0.022 

0.028 

0 .016 

0.019 

0.016 

0.017 

0.000 

0.025 

0.018 

0.029 

0.006 

0.025 

0.030 

0.021 

0.008 

38.7 

Serum# 

175 

0.033 

0.030 

0.021 

0.057 

0.030 

0.038 

0.034 

0. 048 

0. 030 

0. 045 

0.027 

0.031 

0.027 

0.029 

0.067 

0. 041 

0. 038 

0. 033 

0.017 

0.031 

0. 043 

0.035 

0.012 

33.3 

Serum# 

176 

0.1 

-7.8 

-0.8 

-1. 7 

-5.8 

16.1 

12.3 

-4.0 

8.6 

62.4 

-9.7 

-16.2 

-13.8 

-18.1 

6.4 

2 .14 

0.20 

9.2 

Serum# 

176 

0.016 

0.015 

0.011 

0.020 

0.010 

0. 013 

0.016 

0. 019 

0.012 

0.019 

0.014 

0.018 

0.011 

0.017 

0.000 

0.021 

0.017 

0.024 

0.006 

0.013 

0.026 

0.015 

0. 005 

37.5 

Serum# 

177 

0 .4 

-19.6 

-0.7 

3 .1 

-5.8 

17.3 

6. 5 

-2. 3 

2.1 

-3.3 

3.88 

0.15 

3.9 

Serum# 

177 

0 .125 

0.083 

0. 066 

0. 089 

0 .100 

0.097 

0.104 

0.127 

0.080 

0 .155 

0.067 

0.075 

0.095 

0.163 

0 .126 

0 .125 

0.103 

0. 030 

29. 0 

B7
 
Table 7. Round Robin XXVII 

Lab# 

NIST 3 

AVG 

SD 

RSD 

173 

a.a27 

a.al4 

a.ass 

a.a59 

a.al5 

a.al5 

a.a31 

a.a21 

67.7 

Retinyl Palmitate 

174 

a.al6 

a.a58 

a.a65 

a.a14 

a.a38 

a.a27 

7a.6 

175 

o.aa8 

a. a41 

a.a62 

a.aa9 

o.a3a 

o.a26 

87.6 

Table 9. Round Robin XXVII 

Lycopene (Total) 

Lab# 

NIST 3 

AVG 

SD 

RSD 

173 

a.425 

a.33a 

a.239 

a.3S6 

a.691 

0.75a 

a.417 

a.386 

a.426 

a .411 

a.226 

a .499 

a.408 

a.276 

a .421 

a .449 

a .431 

a.4a3 

a .241 

a.387 

a.Sl2 

a.4a9 

a.131 

32. a 

174 

a.S93 

a.432 

a.278 

a.497 

a. 896 

l.12a 

a.S64 

a.S62 

a.S78 

a.SS7 

a.3a3 

a. 7a2 

a. 572 

a.342 

a.571 

a.543 

a.378 

a.633 

a.23a 

a.S29 

a. 645 

a.544 

a.2a6 

37.8 

175 

a.477 

a.344 

a.225 

0.368 

0.789 

0.8la 

a.446 

0.471 

0.4la 

0.418 

0.232 

0.5a7 

0.4a9 

0 .333 

a.428 

0.456 

0.424 

0.446 

0 .27a 

0.414 

0.525 

0.434 

0.147 

34.a 

176 

a .2a4 

a.228 

a.146 

a.162 

a.151 

a.186 

a.187 

0.198 

0.246 

0.154 

a.190 

o.a34 

17.8 

176 

a.186 

0.154 

0.087 

0.159 

a.326 

a.3ao 

a.17a 

o.21a 

0.176 

a.186 

a .118 

a.219 

0.158 

0.149 

a.171 

a.242 

a.251 

0.165 

0.114 

0.176 

0.233 

a.186 

a.a59 

31. 8 

177 

0.024 

a.028 

a.075 

a. 071 

0.168 

a. 025 

a.073 

a.058 

79. 2 

177 

0.354 

0.248 

0.167 

a. 312 

0.542 

0.61a 

0.376 

0.392 

0.3a9 

a.342 

0.186 

a.295 

0.276 

a. 364 

a.438 

0.451 

0. 347 

0.119 

34.2 

Table 8. Round Robin XXVII 

Lute in 

Lab# 

NIST 3 

AVG 

SD 

RSD 

173 

o.a93 

o.1a9 

O.la7 

0.113 

0.122 

0.093 

0.200 

0.138 

O.la4 

0.122 

o.a35 

28.6 

174 

a.a77 

o.a8o 

a.1aa 

a.a86 

a.1a5 

a.074 

0.156 

0.104 

a.085 

a.098 

o.a27 

27.2 

Table la.Round Robin XXVII 

Zeaxanthin 

Lab# 

NIST 

AVG 

SD 

RSD 

173 

o.a42 

0. 04a 

0.036 

0.142 

0.073 

0.048 

0. 046 

0.046 

0.061 

0.038 

61.6 

174 

a.a3a 

0. a22 

o.a22 

a .111 

a.a64 

a.a32 

a.a32 

a.036 

o.a45 

a.a32 

72 .6 

175 

a.097 

a.1aa 

a.109 

0 .lla 

a.123 

a.1a4 

0.178 

0.162 

a.1a3 

0.123 

a.a30 

24.8 

175 

a.042 

a.a38 

o.a32 

a.146 

o.a65 

0.045 

0. a43 

o.a46 

a.059 

0.04a 

67.9 

176 

o.a46 

a.043 

0.053 

a.052 

a.066 

0.037 

a.a85 

a.064 

a.047 

0.056 

a.015 

27.6 

176 

a.022 

a.a28 

a.022 

0.066 

0.048 

a.035 

0. 021 

a. a28 

o.a35 

0.017 

49.a 

177 

0.079 

0.073 

a.097 

a.090 

a.a82 

a.085 

a.all 

12.7 

177 

0. a29 

0. a3a 

a.a26 

0.113 

0.036 

0. a49 

o.a42 

85.4 

B8
 
Table 11.Round Robin XXVII 

Lutein + Zeaxanthin 

Lab# 173 174 175 

0.150 0.109 0.153 

0.185 0.153 0.199 

0.195 0.147 0.195 

0 .203 0.201 0.235 

0.141 0.108 0.175 

0.151 0 .116 0.157 

AVG 0 .171 0.139 0.186 

SD 0.027 0.036 0.031 

RSD 15.6 25.9 16.5 

Table 13.Round Robin XXVII 

Lycopene (Trans) 

Lab# 173 174 175 

0.223 0.294 0.235 

0.354 0.498 0.457 

NIST 3 0.192 0.249 0 .205 

AVG 0.289 0.396 0.346 

SD 0.093 0.144 0.157 

RSD 32.1 36.4 45.4 

Table 15.Round Robin XXVII 

Trans-Alpha-Carotene 

Lab# 173 174 175 

NIST 0.041 0.018 0.027 

176 

0.074 

0.075 

0.085 

0.112 

0.070 

0. 072 

0.081 

0.016 

19.5 

176 

0.111 

0.238 

0.109 

0.175 

0.090 

51.5 

176 

0.016 

177 

0.111 

0 .167 

0.148 

0.201 

0.148 

0.155 

0. 033 

21.l 

177 

0.174 

0.162 

0.174 

177 

0.080 

Table 12.Round Robin XXVII 

Beta-Cryptoxanthin 

Lab# 173 174 175 176 

0.102 0.063 0.065 0. 049 

0.097 0.066 0.068 0.044 

0.115 0.084 0.083 0.054 

0.148 0.123 0.122 0.077 

0.126 0.103 0.095 0. 072 

0. 059 0.040 0.036 0.029 

0.113 0.092 0. 094 0.057 

0.064 0.045 0.040 0. 025 

0.229 0.209 0.186 0.157 

0. 040 0.021 0 .240 0.025 

0.093 0.061 0.064 0.043 

NIST 3 0.058 0. 041 0.042 0.032 

AVG 0 .108 0.082 0.099 0.057 

SD 0. 051 0.051 0.062 0.037 

RSD 47.3 62.2 62.9 65.0 

Table 14.Round Robin XXVII 

Total Cis-Beta-Carotene 

Lab# 173 174 175 

0. 047 0.017 0.033 

Table 16.Round Robin XXVII 

Delta-Tocopherol 

Lab# 173 174 175 

NIST 3 0.212 0.117 0.057 

176 

0.020 

176 

0 .136 

177 

0.064 

0.063 

0.083 

0 .136 

0.080 

0. 036 

0.099 

0. 040 

0. 080 

0.032 

39.4 

177 

177 

0.156 

B9
 
lnterlaboratory S:tecision vs Time 

Retinal 

Percent 

30 

+++ 

I 

20 

+ 

+ 

10 + -------- -- ................ + ............ +-........ . 

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

DATE 0 

.... 

,.. 

Controls Available 

B10
 
lnterlaboratory 1-fecision vs Time 

Alpha-Tocopherol 

Percent 

30 

* 

20 . . . . * . * ......... . - - - - - - - - -

* 

10 * 

* * * * * * * * * * * * * * 

fDATIE 0 

.... 

,, 

B11 
lnterlaboratory Precision vs Time 

Beta-Carotene 

Percent 

30 

x 

20 

x x x 

x x 

x x x x x 

10 --------- z --- - ----- K---- Z Z x ___________ "\? "f::::,:----- ----

x 

IDJATIE 0 3/88 10/88 4/87 7/87 1/88 7/88 9/88 1/89 4/89 8/89 1190 5/9o 9/9o 1191 5/91 8/91 1192 5/92 8/92 1/93 

... 

,... 

Controls Available 

B12
 
 

 

Appendix C. Representative “Individualized Report” for RR27 

Each participant in RR27 received graphical summaries of their own measurement 

performance for total retinol, α-tocopherol, and/or total β-carotene. In RR27, 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 1/93. 

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

just the sera distributed in RR27. 

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

C1
 
Percent ·Blas 

Laboratory FSV-BA 

Retlnol 

30.--~~~~~~~~~~~~~~~

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

10 

0 

·10 

-20 

-30 7117 t/11 7/H 1/11 1/11 4/81 8/H t/ID l/IO 8/ID 1/11 5/11 1/11 1/H 5/12 

% Blas ••om Assigned Values 

C

2
Percent Blas 

Laboratory FSV-BA 

Alpha-Tocopherol 

30r-------~~~~~~~~~~~~~

20 . ... ... ..... .... .. _ ........ .... . . .... - ...... . . ... ........... . 

10 -·· ··-···· -- ····- ·· ··· -- ·· ··--"' ·· · ·- · ·· - · -·· · --

0 

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

. -20 .. ............ · ·····- - ·· ·· - ··· - ····· · · ·· ·-·· ··-- -·· -- · ···· - ·

•30 7/17 1/.. 7/H 1/H 1/89 4/11 11/118 1/IO 5/10 8/80 1 /11 5/81 1/91 I /H 5/92 

% Blas •·om Assigned Values 

C

3
Percent 'Blas 

Laboratory FSV-BA 

Total Beta-Carotene 

30r-----..w--~~~--~~~~~~~~~~~

20 

10 

-10 

-20 

·30 7117 1/81 7/18 1/11 1/11 4/81 ., .. 1/10 1/80 t/10 1/11 5/91 1/11 1/H 5/IZ 

% Bia• • .. om Assigned Values 

C

4
% Bias 

30 

20 - 4:· •. 

10 

0 

-10 

-20 

-30 

Serum II 149 

5/91 

Laboratory FS,V-B

Blind Duplicate Performance 

Retinal 

159 

8/91 

173 

1/93 

155 

8/91 

174 

1/93 

156 

'91 

175 

1/93 

171 

6/92 

176 

1/93 

150 

5/91 

C

5
%Bias 

30 

20 

10 

0 

-10 

-20 .. 

~ '· 

-30 

Serum# 149 

Laboratory FSV-

Blind Duplicate Performance 

Alpha-Tocopherol 

159 173 

.. · 

,. - .. ·: .. . ..... ., 

·:= 

~ . ": i ;-; . 

.. .. 

171 176 

... - . 

:...!:~·

It :F·= •

;• 

150 

5/91 8/91 1{93 

155 

8{91 

174 

1/93 

156 

R/91 

175 

1/93 8/92 1/93 5/91 

C

6
o/o Bias 

30 !'.:., 

20 

10 

.· 

0 

-10 

-20 

':~. I ' '::: ~ •· 

Laboratory FSV-

Blind Duplicate Performance 

Total Beta-Carotene 

. . '"' . . .... 

:-h." 

.. 

.7!~ - 

••• •• 

: ·. :;·;

... ,•; . 

-30 .. ; . :·. ~~ ·: .: ... 

Serum '# 149 159 

5/91 8/91 

173 

1/93 

155 174 

8/91 1 /93 

156 175 

8/91 1/93 

171 176 

8/92 1/93 

150 

5/9

C

7
 

 

 

Appendix D. Updated “All-Lab Report” for RR27 

The following six pages are a modified version of an “All-Lab” report for RR27. 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 lists values for all analytes reported by only once. This page also 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 RR27 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 RR27. 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 NISTa and NISTb in this modified All-Lab report are 

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

D1
 
 

Round Robin XXVII Laboratory Results 

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

Lab 173 174 175 176 177 

FSV-BA 0.506 0.545 0.397 0.528 0.621 

FSV-BD 0.525 0.570 0.431 0.597 0.704 

FSV-BE 0.498 0.554 0.405 0.536 0.712 

FSV-BF 0.491 0.556 0.418 0.542 0.653 

FSV-BG 0.552 0.538 0.377 0.691 0.673 

FSV-BH 0.505 0.527 0.422 0.576 0.675 

FSV-BI 0.449 0.450 0.366 0.503 0.538 

FSV-BJ 0.495 0.528 0.386 0.538 0.661 

FSV-BK 0.533 0.576 0.419 0.547 0.652 

FSV-BL 0.540 0.597 0.562 0.588 0.695 

FSV-BM 0.502 0.554 0.394 0.537 

FSV-BN 0.463 0.467 0.347 0.481 

FSV-BO 0.529 0.624 0.467 0.572 

FSV-BP 0.557 0.585 0.449 0.581 

FSV-BQ 0.480 0.500 0.390 0.530 

FSV-BR 0.503 0.532 0.403 0.541 

FSV-BT 0.580 0.561 0.401 0.534 

FSV-BX 

FSV-BY 0.493 0.527 0.405 0.536 0.644 

FSV-BZ 

FSV-CA 0.499 0.585 0.368 0.513 0.624 

FSV-CB 0.671 0.756 0.508 0.737 

FSV-CH 0.596 0.673 0.473 0.676 0.745 

FSV-CJ 0.583 0.644 0.390 0.613 0.750 

FSV-CK 0.452 0.589 0.386 0.531 0.630 

FSV-CM 

FSV-CO 0.465 0.508 0.367 0.517 0.609 

FSV-CP 0.508 0.538 0.440 0.552 0.692 

FSV-CQ 0.381 0.480 0.355 0.476 0.496 

FSV-CR 0.500 0.540 0.420 0.610 

FSV-CT 0.504 0.577 0.429 0.513 

FSV-CU 0.482 0.509 0.375 0.506 0.611 

FSV-CV 0.491 0.500 0.383 0.501 

FSV-CY 0.500 0.320 0.380 0.540 0.640 

FSV-DC 0.524 0.572 0.414 0.561 0.694 

FSV-DJ 0.880 0.920 0.710 0.860 

FSV-DL 0.352 0.383 0.322 0.398 1.119 

FSV-DM 0.432 0.454 0.346 0.456 0.570 

FSV-DS 0.480 0.550 0.410 0.490 

FSV-DX 0.456 0.489 0.366 0.486 

FSV-DY 0.521 0.530 0.414 0.580 0.718 

FSV-EA 0.468 0.513 0.382 0.537 

FSV-EB 0.514 0.538 0.396 0.541 0.720 

FSV-EC 0.448 0.491 0.366 0.478 

FSV-EI 0.285 0.298 0.245 0.345 

FSV-EJ 0.497 0.523 0.407 0.519 0.643 

FSV-EK 0.571 0.613 0.415 0.595 

FSV-EX 0.430 0.460 0.350 0.460 

FSV-FF 0.505 0.530 0.401 0.584 

173 174 175 176 177 

0.055 0.058 0.041 0.162 0.075 

0.014 nd nd 0.146 0.028 

nd nd nd 0.151 nd 

nd nd nd 0.228 nd 

nd nd nd 0.186 0.071 

0.015 nq nq 0.198 

0.015 0.014 0.009 0.246 

0.027 0.016 0.008 0.204 0.024 

0.059 0.065 0.062 0.187 0.168 

nd nd nd 0.203 

173 174 175 176 177 

10.34 7.45 10.01 5.13 16.2 

11.70 7.98 10.40 6.10 17.0 

11.42 7.90 11.00 5.20 17.2 

11.12 7.84 10.71 5.13 15.5 

10.65 7.24 9.50 5.70 15.7 

11.04 7.63 10.24 5.15 17.2 

9.71 6.52 9.31 4.61 13.2 

11.15 7.71 10.76 4.94 16.2 

10.05 7.04 9.00 4.49 13.9 

11.35 7.61 10.54 5.14 16.6 

10.85 7.80 10.50 5.20 

11.18 8.09 10.03 6.17 

13.01 9.66 11.30 5.00 

11.96 7.97 11.42 5.62 

10.00 6.50 10.20 4.50 

11.63 8.39 11.25 5.43 

10.40 7.35 10.08 4.93 16.0 

9.58 6.30 10.80 3.69 19.2 

9.12 7.38 8.69 3.95 14.4 

8.41 5.83 7.02 4.74 

11.30 8.14 10.10 3.64 14.5 

10.14 7.00 9.13 4.73 15.7 

10.10 8.99 11.00 5.55 17.0 

11.40 7.30 10.30 5.00 16.3 

10.26 7.10 9.57 4.53 15.0 

7.66 5.45 7.08 3.40 11.6 

10.67 7.61 9.50 4.84 15.1 

10.80 7.60 10.40 4.80 

8.24 6.05 8.95 4.31 

10.11 7.33 9.56 5.02 15.8 

10.90 7.92 9.77 5.28 

10.50 4.53 10.57 4.93 15.6 

15.90 10.70 16.70 7.20 

8.70 6.46 8.12 3.64 13.7 

10.32 7.65 9.06 4.78 

10.30 9.00 11.00 6.30 

7.84 4.70 8.40 3.58 

11.10 7.67 10.15 4.91 14.4 

9.54 6.70 8.93 4.50 

8.73 6.15 8.58 4.25 

10.95 7.76 10.73 4.36 16.2 

10.33 7.27 10.02 4.88 

10.54 7.57 10.02 4.78 

173 174 175 176 177 

2.64 2.15 1.88 2.01 3.65 

2.90 2.40 2.10 2.10 4.00 

2.70 2.32 1.94 2.12 3.85 

3.20 2.58 2.23 2.48 4.55 

2.55 2.00 1.78 1.97 3.12 

2.95 2.22 2.03 2.05 3.79 

2.18 1.76 1.53 1.84 

3.02 2.50 2.13 2.27 

2.83 2.24 1.97 2.14 3.90 

2.94 2.35 2.06 3.47 3.96 

2.82 2.85 2.11 2.40 4.13 

3.09 2.70 2.18 2.32 

2.27 1.76 1.69 1.79 

2.19 1.77 1.33 1.75 

2.77 2.28 1.90 1.93 3.75 

3.17 2.61 2.16 2.49 

n 46 46 46 46 26 6 4 4 10 5 43 43 43 43 25 16 16 16 16 10 

Min 0.285 0.298 0.245 0.345 0.496 0.014 0.014 0.008 0.146 0.024 7.66 4.53 7.02 3.40 11.6 2.18 1.76 1.33 1.75 3.12 

Mean 0.504 0.541 0.406 0.546 0.673 0.031 0.038 0.030 0.191 0.073 10.49 7.37 10.01 4.88 15.6 2.76 2.28 1.94 2.20 3.87 

Max 0.880 0.920 0.710 0.860 1.119 0.059 0.065 0.062 0.246 0.168 15.90 10.70 16.70 7.20 19.2 3.20 2.85 2.23 3.47 4.55 

SD 0.084 0.097 0.067 0.082 0.109 0.021 0.027 0.026 0.032 0.058 1.40 1.14 1.47 0.76 1.5 0.33 0.33 0.25 0.41 0.36 

CV 17 18 16 15 16 68 71 88 17 79 13 16 15 16 10 12 15 13 19 9 

NISTa 0.517 0.542 0.407 0.562 0.632 10.76 7.48 9.77 4.72 15.8 2.96 2.42 1.94 2.13 3.85 

NISTb 0.482 0.502 0.372 0.547 0.643 nd nd nd 0.154 0.025 10.53 7.96 10.28 5.03 15.8 2.77 2.23 1.98 2.27 3.87 

Median 0.500 0.538 0.399 0.537 0.657 0.021 0.193 0.071 10.50 7.57 10.08 4.91 15.7 2.83 2.30 2.00 2.11 3.87 

eSD 0.040 0.056 0.032 0.053 0.056 0.010 0.031 0.064 0.92 0.61 0.96 0.55 1.2 0.28 0.35 0.19 0.29 0.19 

eCV 8 10 8 10 8 46 16 90 9 8 10 11 8 10 15 9 14 5 

D2
 

All Lab Report Page 1 / 6 
Round Robin XXVII Laboratory Results 

Lab 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BT 

FSV-BX 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CH 

FSV-CJ 

FSV-CK 

FSV-CM 

FSV-CO 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CT 

FSV-CU 

FSV-CV 

FSV-CY 

FSV-DC 

FSV-DJ 

FSV-DL 

FSV-DM 

FSV-DS 

FSV-DX 

FSV-DY 

FSV-EA 

FSV-EB 

FSV-EC 

FSV-EI 

FSV-EJ 

FSV-EK 

FSV-EX 

FSV-FF 

n 

Min 

Mean 

Max 

SD 

NISTa 

NISTb 

Median 

eSD 

eCV 

Total β-Carotene, μg/mL 

173 174 175 176 177 

0.96 0.377 0.87 0.410 2.26 

1.13 0.490 1.04 0.480 3.07 

0.92 0.355 0.97 0.412 2.39 

0.83 0.300 0.73 0.324 2.03 

1.02 0.421 0.92 0.435 2.50 

0.85 0.332 0.77 0.361 1.82 

0.93 0.348 0.85 0.429 2.46 

0.89 0.570 0.79 0.485 

0.37 0.145 0.43 0.196 

1.07 0.231 1.00 0.401 

1.76 1.330 2.31 1.040 

0.99 0.379 0.89 0.424 

0.93 0.386 0.82 0.386 2.29 

0.96 0.387 0.97 0.442 2.58 

0.95 0.377 0.98 0.416 

0.85 0.341 0.73 0.335 1.90 

1.38 0.481 1.28 0.528 2.95 

0.93 0.428 1.02 0.504 2.86 

0.96 0.410 0.86 0.412 2.36 

0.70 0.296 0.64 0.294 1.63 

0.84 0.275 0.72 0.204 1.83 

0.99 0.383 0.93 0.382 

0.79 0.325 0.64 0.350 1.96 

1.13 0.464 0.98 0.477 

0.93 0.300 0.90 0.470 2.88 

0.98 0.369 0.87 0.406 2.42 

0.86 0.344 0.63 0.463 2.21 

0.72 0.309 0.72 0.316 2.04 

0.84 0.423 0.82 0.376 

0.71 0.300 0.72 0.330 

0.87 0.361 0.81 0.412 2.35 

0.33 0.089 0.35 0.171 

0.93 0.372 0.93 0.434 2.53 

0.71 0.300 0.63 0.305 

0.90 0.371 0.79 0.340 

1.12 0.395 1.00 3.19 

0.80 0.478 0.79 0.332 

0.87 0.330 0.89 0.410 

0.91 0.389 0.83 0.422 

39 39 39 38 23 4 4 4 4 3 4 4 4 4 3 20 19 21 19 15 

0.33 0.089 0.35 0.171 1.63 0.726 0.293 0.599 0.313 1.836 0.047 0.017 0.033 0.020 0.127 0.023 0.006 0.017 0.006 0.066 

0.91 0.384 0.87 0.403 2.37 0.880 0.349 0.787 0.374 2.084 0.060 0.027 0.044 0.031 0.156 0.052 0.022 0.035 0.015 0.103 

1.76 1.330 2.31 1.040 3.19 0.957 0.396 0.877 0.404 2.362 0.069 0.032 0.052 0.037 0.204 0.089 0.035 0.067 0.024 0.163 

0.23 0.178 0.29 0.134 0.42 0.106 0.043 0.128 0.043 0.264 0.009 0.007 0.008 0.007 0.042 0.015 0.007 0.012 0.004 0.030 

25 46 33 33 18 12 12 16 11 13 16 27 18 24 27 28 30 33 29 29 

0.89 0.315 0.69 0.322 1.95 

0.87 0.343 0.78 0.413 2.22 

0.92 0.371 0.85 0.410 2.36 

0.10 0.068 0.17 0.084 0.48 

11 18 21 20 21 

trans-β-Carotene, μg/mL 

173 174 175 176 177 

0.895 0.345 0.814 0.376 2.055 

0.957 0.396 0.877 0.403 2.362 

0.942 0.362 0.856 0.404 

0.726 0.293 0.599 0.313 1.836 

0.862 0.312 0.659 0.288 1.760 

0.786 0.311 0.731 0.374 2.000 

Total cis-β-Carotene, μg/mL 

173 174 175 176 177 

0.069 0.032 0.052 0.034 0.204 

0.063 0.025 0.046 0.032 0.138 

0.047 0.017 0.033 0.020 

0.060 0.032 0.045 0.037 0.127 

0.030 0.003 0.034 0.034 0.190 

0.082 0.032 0.051 0.039 0.220 

Total α-Carotene, μg/mL 

173 174 175 176 177 

0.054 0.022 0.038 0.013 0.097 

0.050 0.020 0.030 0.010 0.100 

0.065 0.022 0.057 0.020 0.089 

0.050 0.017 0.034 0.016 0.104 

0.048 0.021 0.030 0.015 0.083 

0.036 0.016 0.027 0.014 0.067 

0.049 0.029 0.033 0.024 

0.023 0.006 0.017 0.006 

0.055 0.018 0.038 0.017 

0.048 0.025 0.031 0.013 

0.042 0.022 0.030 0.012 0.080 

0.047 0.026 0.033 0.016 0.125 

0.089 nd 0.067 nd 0.163 

0.049 0.035 0.021 0.011 0.066 

0.062 0.031 0.048 0.019 0.127 

0.040 0.016 0.027 0.011 0.075 

0.053 0.019 0.031 0.018 

0.038 0.017 0.029 0.017 0.095 

nd nd 0.030 nd nd 

0.079 0.028 0.045 0.019 0.155 

0.059 0.025 0.041 0.021 0.126 

0.068 0.030 0.043 0.026 0.125 

0.050 0.022 0.031 0.016 0.097 

0.010 0.006 0.006 0.004 0.033 

19 27 18 28 34 

D3
 

All Lab Report Page 2 / 6 

CV 
 

Round Robin XXVII Laboratory Results 

Total Lycopene, μg/mL trans-Lycopene, μg/mL 

Lab 173 174 175 176 177 173 174 175 176 177 

FSV-BA 

FSV-BD 

FSV-BE 0.75 1.12 0.81 0.300 0.61 

FSV-BF 0.69 0.90 0.79 0.326 0.54 

FSV-BG 0.24 0.28 0.23 0.087 0.17 

FSV-BH 0.42 0.56 0.45 0.170 0.38 

FSV-BI 0.33 0.43 0.34 0.154 0.25 

FSV-BJ 0.23 0.30 0.23 0.118 0.19 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 0.24 0.23 0.27 0.114 

FSV-BP 0.43 0.38 0.42 0.251 

FSV-BQ 

FSV-BR 

FSV-BT 0.39 0.53 0.41 0.176 

FSV-BX 0.43 0.58 0.41 0.176 0.31 

FSV-BY 0.43 0.59 0.48 0.186 0.35 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CH 0.42 0.57 0.43 0.171 0.36 

FSV-CJ 0.36 0.50 0.37 0.159 0.31 

FSV-CK 0.39 0.56 0.47 0.210 0.39 

FSV-CM 

FSV-CO 

FSV-CP 0.41 0.57 0.41 0.158 0.29 

FSV-CQ 

FSV-CR 

FSV-CT 

FSV-CU 

FSV-CV 0.50 0.70 0.51 0.219 

FSV-CY 

FSV-DC 

FSV-DJ 

FSV-DL 0.28 0.34 0.33 0.149 0.28 

FSV-DM 

FSV-DS 

FSV-DX 

FSV-DY 0.41 0.56 0.42 0.186 0.34 

FSV-EA 

FSV-EB 

FSV-EC 

FSV-EI 0.40 0.63 0.45 0.165 

FSV-EJ 0.45 0.54 0.46 0.242 0.44 

FSV-EK 0.34 0.48 0.37 0.138 

FSV-EX 

FSV-FF 

n 21 21 21 21 15 

Min 0.23 0.23 0.23 0.087 0.17 

Mean 0.41 0.54 0.43 0.184 0.35 

Max 0.75 1.12 0.81 0.326 0.61 

SD 0.13 0.20 0.14 0.058 0.12 

CV 32 37 33 32 34 

NISTa 

NISTb 0.51 0.65 0.53 0.233 0.45 

Median 0.41 0.56 0.42 0.171 0.34 

eSD 0.06 0.11 0.07 0.033 0.07 

eCV 15 20 18 19 22 

0.223 0.294 0.235 0.111 0.174 

0.354 0.498 0.457 0.238 

0.240 0.330 0.260 0.120 

3 3 3 3 1 

0.223 0.294 0.235 0.111 

0.272 0.374 0.317 0.156 0.174 

0.354 0.498 0.457 0.238 

0.071 0.109 0.122 0.071 

26 29 38 45 

0.192 0.249 0.205 0.109 0.162 

Total β-Cryptoxanthin, μg/mL 

173 174 175 176 177 

0.097 0.066 0.068 0.044 0.063 

0.115 0.084 0.083 0.054 0.083 

0.102 0.063 0.065 0.049 0.064 

0.229 0.209 0.186 0.157 

0.040 0.021 0.240 0.025 

0.064 0.045 0.040 0.025 

0.093 0.061 0.064 0.043 

0.126 0.103 0.095 0.072 0.080 

0.084 0.060 0.062 0.040 0.068 

0.095 0.078 0.078 0.044 0.083 

0.148 0.123 0.122 0.077 0.136 

0.059 0.040 0.036 0.029 0.036 

0.113 0.092 0.094 0.057 0.099 

0.121 0.080 0.086 nd 

14 14 14 13 9 

0.040 0.021 0.036 0.025 0.036 

0.106 0.080 0.094 0.055 0.079 

0.229 0.209 0.240 0.157 0.136 

0.045 0.045 0.056 0.035 0.028 

43 56 59 63 35 

0.058 0.041 0.042 0.032 0.040 

0.100 0.072 0.081 0.044 0.080 

0.027 0.024 0.024 0.019 0.024 

28 33 29 44 30 

D4
 

All Lab Report Page 3 / 6 
 

Round Robin XXVII Laboratory Results 

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

Lab 173 174 175 176 177 173 174 175 176 177 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BT 

FSV-BX 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CH 

FSV-CJ 

FSV-CK 

FSV-CM 

FSV-CO 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CT 

FSV-CU 

FSV-CV 

FSV-CY 

FSV-DC 

FSV-DJ 

FSV-DL 

FSV-DM 

FSV-DS 

FSV-DX 

FSV-DY 

FSV-EA 

FSV-EB 

FSV-EC 

FSV-EI 

FSV-EJ 

FSV-EK 

FSV-EX 

FSV-FF 

n 

Min 

Mean 

Max 

SD 

CV 

NISTa 

NISTb 

Median 

eSD 

eCV 

173 174 175 176 177 

0.040 0.022 0.038 0.028 0.030 

0.042 0.030 0.042 0.022 0.029 

0.073 0.064 0.065 0.048 

>0.046 >0.032 >0.043 >0.021 

0.036 0.022 0.032 0.022 0.026 

0.142 0.111 0.146 0.066 0.113 

0.048 0.032 0.045 0.035 

0.090 nd nd nd 

0.195 0.147 0.195 0.085 0.148 

0.107 0.100 0.109 0.053 0.097 0.147 0.122 0.147 0.081 0.127 

0.109 0.080 0.100 0.043 0.073 0.150 0.109 0.153 0.074 0.111 

0.122 0.105 0.123 0.066 0.151 0.116 0.157 0.072 

0.200 0.156 0.178 0.085 

>0.138 >0.104 >0.162 >0.064 >0.184 >0.136 >0.205 >0.085 

0.113 0.086 0.110 0.052 0.090 0.149 0.108 0.142 0.074 0.116 

0.093 0.077 0.097 0.046 0.079 

0.185 0.153 0.199 0.075 0.167 

0.203 0.201 0.235 0.112 0.201 

0.093 0.074 0.104 0.037 0.141 0.106 0.149 0.072 

0.141 0.108 0.175 0.070 0.148 

0.090 0.090 0.110 0.040 0.180 

0.199 0.147 0.200 0.081 

9 9 9 9 4 7 6 6 6 4 10 9 9 9 

0.090 0.074 0.097 0.037 0.073 0.036 0.022 0.032 0.022 0.026 0.141 0.106 0.142 0.070 0.111 

0.125 0.102 0.126 0.056 0.085 0.067 0.047 0.061 0.037 0.049 0.164 0.130 0.172 0.079 0.145 

0.200 0.156 0.200 0.085 0.097 0.142 0.111 0.146 0.066 0.113 0.203 0.201 0.235 0.112 0.201 

0.043	 0.030 0.037 0.018 0.011 0.038 0.035 0.043 0.017 0.042 0.024 0.032 0.031 0.013 0.032 

35 30 29 31 13 57 75 70 47 85 15 24 18 16 22 

0.104 0.085 0.103 0.047 0.082 0.046 0.036 0.046 0.028 0.036 0.150 0.121 0.149 0.075 0.118 

0.109 0.090 0.110 0.052 0.048 0.031 0.044 0.032 0.151 0.116 0.157 0.074 0.148 

0.024	 0.019 0.015 0.018 0.018 0.013 0.013 0.014 0.014 0.012 0.022 0.004 0.031 

22 21 13 34 37 43 29 45 9 10 14 5 21 

D5
 

All Lab Report	 Page 4 / 6 

7 
Round Robin XXVII Laboratory Results 

Analytes Reported By One Laboratory
 

Values in μg/mL
 

Analyte Code 173 174 175 176 177 

δ-Tocopherol NISTb 0.212 0.117 0.057 0.136 0.156 

trans-α-Carotene NISTb 0.041 0.018 0.027 0.016 0.080 

trans-Lutein FSV-BT 0.138 0.104 0.162 0.064 

trans-Zeaxanthin FSV-BT 0.046 0.032 0.043 0.021 

Legend 

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

nq Not quantitatively determined (i.e., reported as 'trace')
 

>x Value greater than x
 

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
 

All Lab Report Page 5 / 6 
Round Robin XXVII Laboratory Results
 

% Bias Summary
 

Lab TR aT g/bT bC 

FSV-BA -1±3 1±3 -6±1 1±3 

FSV-BD 7±2 10±8 

FSV-BE 2±4 8±2 3±2 25±6 

FSV-BF 1±3 4±3 -1±2 2±7 

FSV-BG 7±13 1±9 -16±4 

FSV-BH 3±4 4±3 14±3 9±3 

FSV-BI -12±5 -10±5 -12±5 -12±6 

FSV-BJ -1±2 4±3 -1±3 1±4 

FSV-BK 4±3 -8±3 

FSV-BL 15±15 5±3 

FSV-BM 1±2 4±1 

FSV-BN -11±3 10±11 -21±5 15±28 

FSV-BO 11±6 16±12 -56±6 

FSV-BP 10±2 12±4 -2±26 

FSV-BQ -4±3 -7±6 169±69 

FSV-BR 0±1 

FSV-BT 5±8 11±0 7±1 4±2 

FSV-BX -2±4 

FSV-BY -1±1 0±2 0±2 8±4 

FSV-BZ -4±19 5±7 

FSV-CA -2±6 -12±6 

FSV-CB 35±6 -19±11 

FSV-CH 20±5 -4±14 15±28 -13±6 

FSV-CJ 12±9 -5±4 37±12 

FSV-CK -2±7 9±8 10±9 16±9 

FSV-CM 3±4 

FSV-CO -6±2 -5±2 3±4 

FSV-CP 4±4 -28±2 -26±4 

FSV-CQ -16±7 -2±3 -25±16 

FSV-CR 5±6 1±2 

FSV-CT 3±6 -16±5 3±7 

FSV-CU -6±1 -2±3 -17±5 

FSV-CV -5±2 3±5 11±4 20±5 

FSV-CY -9±17 -7±19 5±16 

FSV-DC 5±1 2±3 

FSV-DJ 71±8 51±10 

FSV-DL -7±43 -7±14 

FSV-DM -14±1 -18±5 -18±4 

FSV-DS -2±5 -3±5 -2±11 

FSV-DX -9±1 14±13 -19±3 

FSV-DY 5±4 -3±2 

FSV-EA -4±3 -27±9 -18±4 -65±8 

FSV-EB 2±4 0±5 5±4 

FSV-EC -10±1 -10±2 -24±3 

FSV-EI -40±4 -16±2 -24±7 -7±8 

FSV-EJ -1±2 1±7 -4±3 20±12 

FSV-EK 11±5 -2±2 13±4 -3±22 

FSV-EX -14±1 -1±1 -3±7 

FSV-FF 2±4 1±3 

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
 

All Lab Report Page 6 / 6 
 

 

 

Appendix E. Shipping Package Inserts for RR28 

Two items were included in each package shipped to an RR28 participant: 

•	 Cover letter. The original letter has been lost. It would have been similar to the 

reconstructed cover letter for RR27 provided in Appendix A. That is, the cover letter for 

RR28 would likely have: 

o	 described the five samples, 181 to 185 (all lyophilized), distributed in this study; 

o	 provided guidance for reconstituting the samples and recommended a number of 

standard wavelengths and associated E1% cm absorptivities; 

o	 stated that the results were due by June 14, 1993 and should be mailed or faxed to 

Ms. Nancy T. Miles; 

o	 stated that analytical and technical queries should be directed to Willie E. May, PhD; 

o	 stated the date and venue for the 1993 MMQAP Workshop, and 

o	 was signed by Willie E. May, PhD. 

•	 Datasheet. 

These items were attached to the shipping box. 

E1
 
 

 

ROUND ROBIN XXVIII RESULTS FROM LABORATORY # _________ 

DATE OF ANALYSIS ___________ 

RESULTS IN ug/mL 

SAMPLE NUMBER ANALYTE RESULT 

SERUM 181 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 182 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 183 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 184 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 185 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

OPTIONAL ANALYTES: SUPPLY ONE RESULT IF AVAILABLE 

SERUM # 181 182 183 184 185 

TRANS-BETA CAROTENE 

ALPHA-CAROTENE 

RETINYL PALMITATE 

GAMMA-TOCOPHEROL 

LYCOPENE (TOTAL) 

9-CIS-BETA CAROTENE 

13-CIS-BETA-CAROTENE 

LUTEIN 

ZEAXANTHIN 

BETA-CRYPTOXANTHIN 

DIRECTIONS: Reconstitute with 1.0 mL distilled water. 

RESULTS DUE BY: June 14, 1993 

FAX RESULTS TO 301/926-8671 

E2
 
 

 

 

Appendix F. Final Report for RR28 

The following eleven pages are the final report for RR28 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 17 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, trans-lycopene, 

trans-lutein & zeaxanthin, trans-α-carotene, δ-tocopherol, and 

cis-lutein & zeaxanthin. 

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

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

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

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

listing of the RR28 results where the original codes have been altered to ensure 

confidentiality. Appendix H also provides more relevant summary statistics. 

F1
 
F2
F3
F4
 
F5
 
F6
 
F7
 
F8
 
F9
 
F10
 
F11
 
F12
 
 

 

Appendix G. Representative “Individualized Report” for RR28 

Each participant in RR28 received graphical summaries of their own measurement 

performance for total retinol, α-tocopherol, and/or total β-carotene. In RR28, 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 4/93. 

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

just the sera distributed in RR28. 

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

G1
 
Percent Bias 

Laboratory FSV-BA 

Retinol 

20 ,__ ....... --........... --..... ---... -............ . . --. -................ . 

10i--··· · ···--·---······ - ······-·---··············-·····-················ 

-20 

-30 7/87 1188 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 1193 4/93 

% Bias from Assigned Values 

G2
 
Laboratory . FSV-BA 

Alpha-Tocopherol 

Percent Bias 

30 . . 

.:;, ·-

20 .• mpm_ . . • - - . . . . - - . . • . . - . • . . . . . . . . .. . . . . . . . . . . . . . . - • . . . . . . • • • • . . - . • . 

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

-

.. 

0 

-10 Ir.• .. . . .. .. -... ... ""' .. .. .. ... . ... ... ... ... . - ... .. - .. - --.. ... . ... .. ... .. .. ;.·- ... ... . - .. - .. .. ... ... .. - .. .. .. . ... .. ... ... ... ... ... ,,_ .. - .. .. -20 ............ ._ - - - oP.lt• - .................................. - - .......................... ......... "' .............. " ............ "' ... <!- .......... ---30 7/87 1/88 7/88 9/88 1/89 4/89 8/89 1/90 5/90 9/90 1191 5191 8191 1192 5/92 8/92 1/93 4193 

% Bias from Assigned Values 

G3
 
Laboratory · FSV-BA 

Total Beta-Carotene 

Percent Bias 

30 1 mm m 

201-.. 

10 I-•• 

0 IJ rr 

:: 

-10 1-•••... 

• .. ..... ....•• l\i 

1: 

.. ... . . . ... .. .. .. .. . .. . ;: 

.............. _ ................................................ ... ......... ... . 

mil 

,,.1:::1 

• •••••••• .••• •,n; 

;;1w 

fil ] A :: rnm '' '' ; i 

H. ' 

.... 

I'' 'i "I 

! 1 I '•u-, . 'I . l 

. . . ..... ...... -. .. . . .. . .. ..................... 

- -

.. .. . .. ... 

-20 I-............ . ............................. -..... · .................... ............. , _._ ............. ,. ................. ... 

-30 7/87 1188 7 /88 9/88 1 /89 4/89 8/89 1 /90 5/90 9/90 1 /91 6/91 8/91 1 /92 5/92 8/92 1/93 4/93 

% Bias from Assigned Values 

G4
 
Laboratory FSV-BA 

%> Bias 

Blind Duplicate Performance 

Retinol 

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

10· ································-······································ 

01 ! 

-10 . .... - ..... -...................... -.. -... -... -....................... . 

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

Serum # 149 159 173 

5/91 8/91 1/93 

155 174 

8/91 1/93 

156 175 

8/91 1/93 

171 176 150 161 177 182 185 

8/92 1/93 5/91 1/92 1/93 4/93 4/93 

G5
 
%> Bias 

Laboratory FSV-BA 

Blind Duplicate Performance 

Alpha-Tocopherol 

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

10· -························-··· · ·· · ··· · ·- · ·········· · ·- · ··· · · · · · ·· ···· · 

-10 ... . ...... ... . . . . - .... -.... . . - -. .. -" -. . -. --. .. . . -. -- -. - -.... . . -. .. . -.. 

Serum # 149 159 173 155 174 156175 171 176 150161 177 182 185 

5/91 8/91 1/93 8/91 1/93 8/91 1/93 8/92 1/93 5/91 1/92 1/93 4/93 4/93 

G6
 
<M> Bias 

Laboratory FSV-BA. 

Blind Duplicate Performance 

Total Beta-c·arotene 

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

10 .. - ... .. ... .. • .. .. ... .. .. .. . • .. " .... ; ... "' .. ........ .- - ,., - - ... ... -- ... -- ....... .............. ................... .. 

0 

-10 · ··· ······································· ··· ······ ·--·-· ····· ·· ········ 

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

Serum # 149 159 173 155 174 156 175 171 176 150 161 177 182 185 

5/91 8/91 1/93 8/91 1/93 8/91 1/93 8/92 1/93 5/91 1/92 1/93 4/93 4/93 

G7
 
 

 

 

Appendix H. Updated “All-Lab Report” for RR28 

The following six pages are an updated version of an “All-Lab” report for RR28. 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 lists values for all analytes reported by only once. This page also 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 RR28 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 RR28. 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 NISTa and NISTb in this updated All-Lab report are 

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

H1 
Round Robin XXVIII Laboratory Results 

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

Lab 181 182 183 184 185 

FSV-BA 0.488 0.529 0.539 0.348 0.529 

FSV-BD 0.504 0.588 0.594 0.377 0.581 

FSV-BE 0.450 0.499 0.531 0.325 0.510 

FSV-BF 0.493 0.518 0.564 0.337 0.500 

FSV-BG 0.434 0.473 0.475 0.328 0.468 

FSV-BH 0.449 0.497 0.520 0.335 0.518 

FSV-BI 0.428 0.510 0.539 0.338 0.516 

FSV-BJ 0.500 0.555 0.559 0.364 0.561 

FSV-BK 0.545 0.580 0.578 0.376 0.578 

FSV-BL 0.545 0.577 0.594 0.448 0.676 

FSV-BM 0.468 0.536 0.571 0.360 0.539 

FSV-BN 0.487 0.578 0.596 0.386 0.587 

FSV-BO 0.570 0.573 0.581 0.378 0.556 

FSV-BP 0.470 0.550 0.560 0.360 0.550 

FSV-BQ 0.494 0.569 0.606 0.398 0.593 

FSV-BR 0.462 0.510 0.558 0.365 0.531 

FSV-BS 0.604 0.171 0.158 0.080 0.414 

FSV-BT 0.509 0.546 0.564 0.371 0.552 

FSV-BX 0.480 0.546 0.560 0.340 0.531 

FSV-BY 0.455 0.491 0.519 0.324 0.483 

FSV-BZ 

FSV-CA 0.481 0.489 0.528 0.322 0.515 

FSV-CB 0.622 0.693 0.706 0.451 0.687 

FSV-CH 0.593 0.651 0.705 0.450 0.697 

FSV-CJ 0.614 0.620 0.656 0.377 0.661 

FSV-CM 

FSV-CO 0.438 0.484 0.500 0.309 0.482 

FSV-CP 0.469 0.570 0.542 0.348 0.561 

FSV-CR 0.460 0.570 0.580 0.370 0.540 

FSV-CT 0.594 0.643 0.646 0.467 0.648 

FSV-CU 0.454 0.510 0.525 0.339 0.502 

FSV-CV 0.405 0.538 0.533 0.360 0.530 

FSV-CY 0.480 0.560 0.540 0.330 0.520 

FSV-DC 0.484 0.579 0.569 0.361 0.571 

FSV-DJ 0.460 0.590 0.640 0.410 0.610 

FSV-DK 1.100 1.200 0.750 1.220 

FSV-DM 0.430 0.510 0.519 0.323 0.502 

FSV-DS 0.540 0.590 0.580 0.470 0.610 

FSV-DX 0.426 0.515 0.527 0.352 0.506 

FSV-EB 0.505 0.551 0.556 0.369 0.551 

FSV-EC 0.344 0.420 0.416 0.261 0.407 

FSV-EK 0.516 0.576 0.603 0.355 0.595 

FSV-EN 0.270 0.293 0.324 0.202 0.313 

FSV-EX 0.420 0.490 0.490 0.320 0.490 

FSV-FC 0.583 0.667 0.672 0.437 0.658 

FSV-FF 0.539 0.666 0.694 0.492 0.711 

181 182 183 184 185 

0.141 0.070 0.142 0.142 0.067 

0.122 0.068 0.139 0.141 0.059 

0.191 0.079 0.199 0.190 0.078 

0.114 0.088 0.132 0.128 0.077 

0.115 0.041 0.137 0.098 0.050 

0.191 0.102 0.155 0.198 0.063 

0.119 0.072 0.108 0.118 0.068 

0.150 0.102 0.126 0.149 0.086 

181 182 183 184 185 

7.03 5.63 11.50 4.39 5.65 

7.70 6.70 12.40 4.50 5.70 

6.77 4.97 10.88 3.91 4.96 

7.92 5.98 12.43 4.57 5.81 

6.66 4.84 10.11 4.11 4.94 

7.19 5.68 11.33 4.44 5.74 

6.98 5.87 12.22 4.48 5.77 

7.13 5.08 10.52 4.21 5.20 

7.19 5.50 11.09 4.41 5.46 

5.84 5.48 10.39 4.10 5.39 

7.20 5.80 10.90 4.40 5.80 

7.85 6.50 12.81 8.48 6.54 

7.84 5.52 11.40 4.48 5.47 

7.23 5.51 11.61 4.33 5.48 

3.50 3.62 9.00 1.89 2.57 

3.37 3.02 5.00 2.58 3.04 

7.55 5.90 11.80 4.83 5.82 

7.12 5.52 11.32 4.16 5.33 

6.95 5.27 10.54 4.07 5.20 

7.13 5.30 12.10 6.39 6.69 

6.79 5.24 11.72 4.50 5.51 

7.85 6.89 10.21 5.69 6.73 

8.37 5.69 10.90 5.58 7.13 

6.51 5.28 11.18 3.83 5.93 

7.33 5.61 11.35 4.58 5.63 

6.91 5.37 11.24 4.18 5.29 

6.46 5.01 9.48 3.72 4.54 

6.90 5.30 11.30 4.20 5.50 

9.28 7.47 15.52 5.49 6.88 

6.29 5.28 10.81 4.30 5.30 

6.80 5.70 12.38 4.13 5.40 

7.34 5.24 11.90 4.19 5.60 

7.00 5.26 11.30 4.38 5.33 

7.30 5.80 11.30 4.60 6.00 

7.23 10.40 4.20 2.90 

5.96 4.79 9.99 3.76 4.82 

6.52 5.49 10.39 4.23 5.37 

7.10 6.30 13.00 6.00 7.00 

7.52 5.08 11.82 6.06 5.20 

0.26 0.20 0.51 0.15 0.23 

7.32 5.46 4.86 4.29 5.69 

4.15 2.84 6.86 2.08 2.27 

7.39 5.58 11.20 4.48 5.75 

6.14 4.73 9.68 3.70 4.76 

181 182 183 184 185 

2.38 2.50 1.90 1.79 2.52 

2.40 2.50 1.86 1.65 2.51 

2.40 2.47 1.76 1.61 2.40 

2.45 2.69 1.89 1.76 2.73 

2.27 2.68 1.95 1.73 2.63 

2.43 2.42 1.77 1.57 2.47 

2.40 2.56 1.20 1.44 2.68 

0.54 1.11 0.24 0.03 1.20 

2.56 2.82 2.04 1.81 2.78 

2.29 2.48 1.76 1.66 2.50 

2.26 2.47 1.71 1.60 2.50 

1.80 1.61 1.43 1.71 1.93 

2.23 2.39 1.65 1.86 2.64 

2.05 2.23 1.58 1.45 2.18 

2.23 2.50 1.84 1.70 3.42 

2.87 2.99 1.82 2.05 3.15 

1.24 1.39 1.09 0.78 1.05 

2.53 2.74 1.91 1.79 2.75 

n 44 43 44 44 44 8 8 8 8 8 44 43 44 44 44 18 18 18 18 18 

Min 0.27 0.17 0.16 0.08 0.31 0.11 0.04 0.11 0.10 0.05 0.26 0.20 0.51 0.15 0.23 0.54 1.11 0.24 0.03 1.05 

Mean 0.50 0.54 0.57 0.37 0.56 0.14 0.08 0.14 0.15 0.07 6.75 5.29 10.65 4.34 5.26 2.19 2.36 1.63 1.55 2.45 

Max 1.10 0.69 1.20 0.75 1.22 0.19 0.10 0.20 0.20 0.09 9.28 7.47 15.52 8.48 7.13 2.87 2.99 2.04 2.05 3.42 

SD 0.12 0.09 0.13 0.09 0.13 0.03 0.02 0.03 0.03 0.01 1.47 1.15 2.40 1.24 1.29 0.53 0.50 0.43 0.46 0.58 

CV 23 17 24 25 23 23 26 19 23 17 22 22 23 29 25 24 21 26 30 24 

NISTa 0.412 0.509 0.504 0.369 0.501 7.35 5.73 11.68 4.53 5.74 2.57 2.62 1.80 1.76 2.59 

NISTb 0.446 0.524 0.548 0.356 0.526 0.107 0.080 0.154 0.166 0.066 7.03 5.72 11.20 4.41 5.41 2.44 2.70 1.92 1.73 2.60 

Median 0.483 0.550 0.560 0.360 0.545 0.132 0.076 0.138 0.142 0.068 7.11 5.48 11.22 4.32 5.48 2.33 2.49 1.76 1.68 2.52 

eSD 0.050 0.059 0.050 0.038 0.063 0.025 0.015 0.013 0.027 0.013 0.49 0.36 1.02 0.31 0.42 0.15 0.21 0.19 0.16 0.28 

eCV 10 11 9 11 12 19 20 10 19 20 7 6 9 7 8 7 9 11 10 11 

H2
 

All Lab Report Page 1 / 6 
Round Robin XXVIII Laboratory Results 

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

Lab 181 182 183 184 185 

FSV-BA 0.092 0.416 0.428 0.351 0.408 

FSV-BD 

FSV-BE 0.093 0.401 0.395 0.338 0.424 

FSV-BF 0.072 0.436 0.338 0.365 0.428 

FSV-BG 0.066 0.501 0.306 0.442 0.528 

FSV-BH 0.085 0.487 0.444 0.409 0.496 

FSV-BI 0.077 0.433 0.389 0.348 0.438 

FSV-BJ 0.127 0.456 0.399 0.374 0.463 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.091 0.736 0.407 0.271 0.476 

FSV-BO 0.634 0.314 0.228 0.261 0.344 

FSV-BP 0.242 0.408 0.367 0.342 0.360 

FSV-BQ 0.397 0.633 0.577 0.392 0.565 

FSV-BR 

FSV-BS >0.087 >0.255 >0.238 >0.215 >0.294 

FSV-BT 0.077 0.438 0.353 0.345 0.420 

FSV-BX 

FSV-BY 0.078 0.430 0.313 0.337 0.429 

FSV-BZ 0.100 0.600 0.500 0.500 0.770 

FSV-CA 

FSV-CB 

FSV-CH 0.095 0.359 0.288 0.399 0.421 

FSV-CJ 0.065 0.340 0.321 0.250 0.347 

FSV-CM 

FSV-CO 0.103 0.421 0.372 0.347 0.415 

FSV-CP 0.060 0.329 0.277 0.259 0.327 

FSV-CR 

FSV-CT 0.074 0.443 0.402 0.374 0.443 

FSV-CU 0.091 0.402 0.410 0.361 0.401 

FSV-CV 0.068 0.503 0.440 0.418 0.480 

FSV-CY 0.100 0.370 0.300 0.310 0.400 

FSV-DC 0.148 0.478 0.394 0.361 0.454 

FSV-DJ 

FSV-DK 

FSV-DM 0.060 0.388 0.332 0.302 0.365 

FSV-DS 0.050 0.444 0.340 0.354 0.332 

FSV-DX 0.630 0.360 0.340 0.360 

FSV-EB 0.078 0.411 0.407 0.401 0.471 

FSV-EC 0.214 1.330 1.195 0.958 1.223 

FSV-EK 0.071 0.375 0.287 0.289 0.393 

FSV-EN 

FSV-EX 0.150 0.450 0.300 0.370 0.360 

FSV-FC 0.073 0.420 0.341 0.341 0.415 

FSV-FF 0.074 0.532 0.481 0.428 0.533 

181 182 183 184 185 

0.080 0.394 0.384 0.315 0.380 

0.085 0.470 0.425 0.388 0.477 

0.087 0.255 0.238 0.215 0.294 

0.075 0.421 0.336 0.326 0.404 

0.088 0.397 0.401 0.354 0.395 

181 182 183 184 185 

0.012 0.022 0.044 0.036 0.028 

nd 0.017 0.019 0.021 0.019 

0.003 0.017 0.017 0.019 0.016 

0.003 0.005 0.009 0.007 0.006 

n 

Min 

Mean 

Max 

SD 

CV 

32 

0.05 

0.14 

0.63 

0.15 

105 

32 

0.31 

0.47 

1.33 

0.18 

38 

32 

0.23 

0.40 

1.20 

0.16 

41 

31 

0.25 

0.37 

0.96 

0.12 

33 

32 

0.33 

0.46 

1.22 

0.16 

36 

5 

0.07 

0.08 

0.09 

0.01 

7 

5 

0.26 

0.39 

0.47 

0.08 

21 

5 

0.24 

0.36 

0.43 

0.07 

21 

5 

0.22 

0.32 

0.39 

0.06 

20 

5 

0.29 

0.39 

0.48 

0.07 

17 

3 

0.00 

0.01 

0.01 

0.01 

92 

4 

0.01 

0.02 

0.02 

0.01 

48 

4 

0.01 

0.02 

0.04 

0.02 

69 

4 

0.01 

0.02 

0.04 

0.01 

57 

4 

0.01 

0.02 

0.03 

0.01 

53 

NISTa 

NISTb 

0.100 

0.101 

0.385 

0.426 

0.385 

0.398 

0.370 

0.352 

0.409 

0.426 

0.070 0.347 0.344 0.319 0.357 

0.085 0.405 0.371 0.323 0.403 

0.030 

0.016 

0.038 

0.021 

0.041 

0.027 

0.051 

0.029 

0.052 

0.023 

Median 

eSD 

eCV 

0.088 

0.023 

26 

0.432 

0.067 

15 

0.369 

0.066 

18 

0.354 

0.056 

16 

0.423 

0.076 

18 

0.085 0.397 0.384 0.326 0.395 

0.004 0.036 0.061 0.042 0.022 

5 9 16 13 6 

H3

All Lab Report Page 2 / 6 
Round Robin XXVIII Laboratory Results 

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

Lab 181 182 183 184 185 

FSV-BA 0.013 0.014 0.052 0.015 0.013 

FSV-BD 

FSV-BE 0.020 0.010 0.040 0.010 0.020 

FSV-BF nd nd 0.044 0.026 nd 

FSV-BG 

FSV-BH 0.010 0.010 0.043 0.012 0.011 

FSV-BI 0.014 0.016 0.042 0.019 0.016 

FSV-BJ 0.022 0.028 0.045 0.018 0.015 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.020 0.027 0.053 0.015 0.022 

FSV-BO 0.006 0.012 0.024 0.011 0.013 

FSV-BP 0.033 0.032 0.046 0.028 0.027 

FSV-BQ 

FSV-BR 

FSV-BS 

FSV-BT 0.020 0.014 0.036 0.015 0.013 

FSV-BX 

FSV-BY 0.018 0.018 0.037 0.022 0.017 

FSV-BZ 0.020 0.020 0.030 0.010 0.030 

FSV-CA 

FSV-CB 

FSV-CH 0.025 0.019 0.044 0.033 0.024 

FSV-CJ 0.016 0.018 0.034 0.020 0.013 

FSV-CM 

FSV-CO 

FSV-CP 0.010 0.012 0.036 0.013 0.012 

FSV-CR 

FSV-CT 

FSV-CU 

FSV-CV 0.006 0.008 0.043 0.010 0.005 

FSV-CY 

FSV-DC 

FSV-DJ 

FSV-DK 

FSV-DM 

FSV-DS 

FSV-DX 

FSV-EB 

FSV-EC 

FSV-EK 

FSV-EN 

FSV-EX 

FSV-FC 

FSV-FF 

181 182 183 184 185 

0.610 0.280 0.340 0.230 0.290 

0.603 0.248 0.272 0.221 0.271 

0.531 0.222 0.250 0.183 0.222 

0.400 0.205 0.211 0.157 0.208 

0.546 0.251 0.266 0.190 0.257 

0.521 0.470 0.313 0.183 0.303 

0.365 0.198 0.182 0.149 0.192 

0.248 0.154 0.154 0.167 0.165 

0.400 0.178 0.174 0.137 0.167 

0.518 0.240 0.240 0.182 0.236 

0.600 0.320 0.370 0.320 0.620 

0.136 0.193 0.200 0.200 0.243 

0.432 0.208 0.233 0.149 0.210 

0.400 0.180 0.200 0.143 0.176 

0.493 0.280 0.305 0.235 0.275 

0.442 0.173 0.305 0.127 0.171 

181 182 183 184 185 

0.394 0.185 0.211 0.143 0.177 

0.310 0.150 0.170 0.130 0.150 

181 182 183 184 185 

0.080 0.047 0.064 0.068 0.047 

0.095 0.057 0.065 0.086 0.060 

0.064 0.049 0.052 0.074 0.048 

0.073 0.122 0.126 0.140 0.114 

0.065 0.036 0.044 0.061 0.035 

0.080 0.037 0.060 0.054 0.058 

0.070 0.042 0.052 0.066 0.043 

0.066 0.040 0.043 0.057 0.039 

0.084 0.049 0.059 0.065 0.055 

0.049 0.034 0.036 0.050 0.033 

0.026 0.026 0.019 0.014 0.026 

0.117 nd 0.066 0.135 nd 

n 

Min 

Mean 

Max 

SD 

CV 

15 

0.01 

0.02 

0.03 

0.01 

43 

15 

0.01 

0.02 

0.03 

0.01 

41 

16 

0.02 

0.04 

0.05 

0.01 

19 

16 

0.01 

0.02 

0.03 

0.01 

40 

15 

0.01 

0.02 

0.03 

0.01 

40 

16 

0.14 

0.45 

0.61 

0.13 

29 

16 

0.15 

0.24 

0.47 

0.08 

32 

16 

0.15 

0.25 

0.37 

0.06 

25 

16 

0.13 

0.19 

0.32 

0.05 

26 

16 

0.17 

0.25 

0.62 

0.11 

43 

2 

0.31 

0.35 

0.39 

0.06 

17 

2 

0.15 

0.17 

0.19 

0.02 

15 

2 

0.17 

0.19 

0.21 

0.03 

15 

2 

0.13 

0.14 

0.14 

0.01 

7 

2 

0.15 

0.16 

0.18 

0.02 

12 

12 

0.03 

0.07 

0.12 

0.02 

31 

11 

0.03 

0.05 

0.12 

0.03 

52 

12 

0.02 

0.06 

0.13 

0.03 

45 

12 

0.01 

0.07 

0.14 

0.03 

48 

11 

0.03 

0.05 

0.11 

0.02 

46 

NISTa 

NISTb 0.043 0.030 0.062 0.034 0.028 0.772 0.316 0.388 0.283 0.330 0.329 0.170 0.170 0.133 0.170 0.045 0.028 0.033 0.042 0.028 

Median 

eSD 

eCV 

0.018 0.016 0.043 0.015 0.015 

0.006 0.006 0.007 0.007 0.004 

33 37 16 44 30 

0.468 0.215 0.245 0.183 0.229 

0.100 0.053 0.078 0.050 0.065 

21 24 32 27 28 

0.072 0.042 0.056 0.065 0.047 

0.012 0.011 0.015 0.015 0.016 

17 26 27 23 35 

H4

All Lab Report Page 3 / 6 
Round Robin XXVIII Laboratory Results 

Total Lutein, μg/mL 

Lab 181 182 183 184 185 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

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-CR 

FSV-CT 

FSV-CU 

FSV-CV 

FSV-CY 

FSV-DC 

FSV-DJ 

FSV-DK 

FSV-DM 

FSV-DS 

FSV-DX 

FSV-EB 

FSV-EC 

FSV-EK 

FSV-EN 

FSV-EX 

FSV-FC 

FSV-FF 

n 

Min 

Mean 

Max 

SD 

CV 

NISTa 

NISTb 

Median 

eSD 

eCV 

0.081 0.041 0.040 0.081 0.041 

0.069 0.043 0.044 0.085 0.047 

0.041 0.022 0.028 0.039 0.017 

0.068 0.039 0.035 0.066 0.040 

0.050 0.040 0.030 0.050 0.090 

0.060 0.036 0.036 0.066 0.036 

0.070 0.040 0.040 0.080 0.040 

0.135 0.078 0.095 0.129 0.080 

8 8 8 8 8 

0.04 0.02 0.03 0.04 0.02 

0.07 0.04 0.04 0.07 0.05 

0.14 0.08 0.10 0.13 0.09 

0.03 0.02 0.02 0.03 0.02 

40 37 49 36 49 

0.079 0.042 0.044 0.079 0.042 

0.069 0.040 0.038 0.073 0.041 

0.016 0.003 0.007 0.015 0.008 

23 7 18 20 20 

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

181 182 183 184 185 

0.026 0.032 0.019 0.019 0.038 

0.038 0.030 0.025 0.028 0.030 

0.026 0.016 0.018 0.021 0.017 

0.070 nd nd nd nd 

181 182 183 184 185 

0.164 0.091 0.095 0.125 0.088 

0.107 0.073 0.059 0.100 0.079 

0.109 0.080 0.069 0.111 0.079 

0.063 0.052 0.044 0.052 0.052 

0.126 0.089 0.082 0.122 0.088 

0.219 0.104 0.114 0.142 0.109 

0.143 0.087 0.076 0.119 0.092 

0.109 0.074 0.060 0.098 0.070 

0.140 

4 3 3 3 3 9 8 8 8 8 

0.03 0.02 0.02 0.02 0.02 0.06 0.05 0.04 0.05 0.05 

0.04 0.03 0.02 0.02 0.03 0.13 0.08 0.07 0.11 0.08 

0.07 0.03 0.03 0.03 0.04 0.22 0.10 0.11 0.14 0.11 

0.02 0.01 0.00 0.00 0.01 0.04 0.02 0.02 0.03 0.02 

52 34 18 21 37 33 19 30 25 20 

0.039 0.029 0.023 0.025 0.028 0.118 0.071 0.067 0.104 0.070 

0.126 0.084 0.073 0.115 0.084 

0.025 0.013 0.019 0.019 0.010 

20 15 27 16 12 

H5
 

All Lab Report Page 4 / 6 
Round Robin XXVIII Laboratory Results 

Analytes Reported By One Laboratory 

Values in μg/mL 

Analyte Code 181 182 183 184 185 

δ-Tocopherol NISTb 0.157 0.153 0.115 0.067 0.171 

trans-α-Carotene NISTb 0.029 0.023 0.054 0.024 0.022 

trans-Lutein&Zeaxanthin FSV-BT 0.124 0.076 0.070 0.104 0.078 

cis-Lutein&Zeaxanthin FSV-BT 0.096 0.029 0.044 0.038 0.031 

Legend 

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

>x Value greater than x 

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 

H6
 

All Lab Report Page 5 / 6 
Round Robin XXVIII Performance Summary
 

% Bias Summary
 

Lab TR aT g/bT bC 

FSV-BA -3±2 2±2 3±3 3±8 

FSV-BD 6±1 10±7 

FSV-BE -7±2 -7±3 1±3 0±6 

FSV-BF -4±5 9±3 -1±3 -4±9 

FSV-BG -12±3 -8±3 5±24 

FSV-BH -7±2 3±2 7±2 13±9 

FSV-BI -7±3 5±4 5±5 -1±7 

FSV-BJ 2±2 -4±3 -1±4 15±17 

FSV-BK 6±4 0±1 

FSV-BL 14±9 -6±7 

FSV-BM -1±2 2±4 

FSV-BN 5±3 32±36 -7±16 15±34 

FSV-BO 7±7 3±4 102±290 

FSV-BP 0±1 1±1 30±81 

FSV-BQ 7±4 -43±15 100±142 

FSV-BR -3±3 

FSV-BS -43±44 -48±6 -74±20 -29±16 

FSV-BT 2±2 7±3 11±3 -4±5 

FSV-BX -2±2 -1±2 -1±1 

FSV-BY -9±2 -5±2 -2±2 -6±7 

FSV-BZ 15±21 -20±13 42±25 

FSV-CA -7±4 0±4 

FSV-CB 26±1 16±16 

FSV-CH 24±4 16±15 0±7 -4±15 

FSV-CJ 17±9 -3±8 -22±6 

FSV-CM 3±2 

FSV-CO -12±2 -2±1 2±8 

FSV-CP -1±4 -13±4 -26±4 

FSV-CR 1±4 -2±2 

FSV-CT 21±6 32±6 1±10 

FSV-CU -7±1 -5±4 1±7 

FSV-CV -5±6 1±6 -12±2 9±18 

FSV-CY -3±4 1±4 -7±13 

FSV-DC 2±2 -1±2 8±16 19±28 

FSV-DJ 9±8 5±3 

FSV-DK 119±9 -14±22 

FSV-DM -9±2 -13±2 -16±9 

FSV-DS 13±10 -4±4 -14±19 

FSV-DX -7±3 20±15 144±315 

FSV-EB 2±2 8±19 4±11 

FSV-EC -26±2 -96±0 187±31 

FSV-EK 5±4 -10±26 19±9 -16±6 

FSV-EN -44±2 -48±8 -48±8 

FSV-EX -12±1 3±2 9±36 

FSV-FC 21±1 -14±0 9±1 -7±6 

FSV-FF 25±9 17±19 

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. 

H7
 

All Lab Report Page 6 / 6 
 

 

 

 

Appendix I. Shipping Package Inserts for RR29 

Two items were included in each package shipped to an RR29 participant: 

•	 Cover letter. The original letter has been lost. It would have been similar to the 

reconstructed cover letter for RR27 provided in Appendix A. That is, the cover letter for 

RR29 would likely have: 

o	 described the five samples, 186 to 190 (186 to 188 lyophilized, 189 and 190 liquid 

frozen), distributed in this study; 

o	 provided guidance for reconstituting the lyophilized samples and recommended a 

number of standard wavelengths and associated E1% cm absorptivities; 

o	 stated that the results were due by August 30, 1993 and should be mailed or faxed to 

Ms. Nancy T. Miles; 

o	 stated that analytical and technical queries should be directed to Willie E. May, PhD; 

o	 stated the date and venue for the 1993 MMQAP Workshop, and 

o	 was signed by Willie E. May, PhD. 

•	 Datasheet. 

These items were attached to the shipping box. 

I1
 
 

 

 

 

ROUND ROBIN XXIX RESULTS FROM LABORATORY # _________ 

DATE OF ANALYSIS ___________ 

RESULTS IN ug/mL 

SAMPLE NUMBER ANALYTE RESULT 

SERUM 186 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 187 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 188 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 189 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

SERUM 190 RETINOL _____________ 

ALPHA-TOCOPHEROL _____________ 

VIAL # ___ BETA-CAROTENE _____________ 

OPTIONAL ANALYTES: SUPPLY ONE RESULT IF AVAILABLE 

SERUM # 186 187 188 189 190 

TRANS-BETA CAROTENE 

ALPHA-CAROTENE 

RETINYL PALMITATE 

GAMMA-TOCOPHEROL 

LYCOPENE (TOTAL) 

9-CIS-BETA CAROTENE 

13-CIS-BETA-CAROTENE 

LUTEIN 

ZEAXANTHIN 

BETA-CRYPTOXANTHIN 

DIRECTIONS: Serum sample 186, 187 and 188, reconstitute with 1.0 mL distilled water. 

Serum samples 189 and 190 are liquid. 

RESULTS DUE BACK: August 30,, 1993 

FAX RESULTS TO 301/926-8671 

I2
 
 

 

Appendix J. Final Report for RR29 

The following 16 pages are the final report for RR29 as provided to all participants: 

•	 The cover letter of a preliminary report for RR29 that was sent to all participants 

shortly before the 1993 QA Workshop. This preliminary report included a series 

of Tables listing the then-current results and various summary values for total 

retinol, α-tocopherol, total β-carotene, γ/β-tocopherol, trans-β-carotene, total 

α-carotene, retinyl palmitate, total lutein, total lycopene, total zeaxanthin, total 

lutein & zeaxanthin, total β-cryptoxanthin, trans-lycopene, trans-lutein & 

zeaxanthin, trans-α-carotene, and δ-tocopherol. Since the complete results were 

distributed in the following “Summary of 1993 Round Robin Activities”, only the 

cover letter is reproduced here. 

•	 The “Summary of 1993 Round Robin Activities” that was sent to participants in 

November 1993. 

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

β-carotene for the nine Round Robin studies conducted from 1991 through 1993. 

•	 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 RR27 and RR28 Final Reports and so are not 

included here. 

•	 Tables 8 thru 19 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, trans-lycopene, 

trans-lutein & zeaxanthin, trans-α-carotene, δ-tocopherol, and 

cis-lutein & zeaxanthin. 

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

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

Due to the complex formatting used in the Tables 4 thru 19, the originally listed 

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

a complete listing of the RR29 results where the original codes have been altered to 

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

J1
 
 

 

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 

October 28, 1993 

Dear Colleague: 

Attached are the tabular results (Tables 1-16) for Round Robin XXIX. The graphical and 

interlaboratory data will be included in the 1993 Round Robin results review, which you will be 

receiving within four weeks. We apologize for the delay. 

Samples for the first study will be distributed the week of January 17. Results will be due March 

19. Written feedback concerning the study will be provided to you by April 25. 

The second set of samples will be shipped the week of April 25 with results due by June 14 and 

feedback to you July 25. 

The third set of samples will be shipped to you the week of July 25. Results will be due by 

August 30 so that all three exercises can be summarized, critiqued, and discussed at the QA 

Workshop. 

A Round Robin study concerning the analysis of fat-soluble vitamins and carotenoid compounds 

in food will also be scheduled to coincide with the second serum round robin study. Please 

contact Dr. Kathy Sharpless (301/975-3121) to indicate your interest in participating. 

Two Round Robin studies concerning the analysis of ascorbic acid in serum will be conducted. A 

schedule for these studies will be forthcoming. Those interested in joining these studies should 

contact Dr. Sam Margolis at 301/975-3137. 

If you have questions, please contact me at 301/975-3120 or FAX 301/926-8671. 

Sincerely, 

Jeanice Brown Thomas 

Research Chemist 

Organic Analytical Research Division 

Chemical Science and technology Laboratory 

Enclosures 

J2
 
( SUMMARY OF 1993 ROUND ROBIN ACTIVITIES 

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

Round-Robin exercises conducted during 1993. Specifically, this section contains for retinol, 

a-tocopherol, and P-carotene, respectively: graphical information concerning Interlaboratory 

Precision vs Time over the past 7 1/2 years; a summary table of data collected over the past three 

years; tabular presentations of both individual laboratory and summary statistical data for Round 

Robins xxvn, XXVIII, and XXIX; a Blind Control Chart representing a summary of each 

laboratory's data vs assigned values for the past six years; a graphical presentation of data from 

each laboratory's analysis of blind replicate samples over the past three years. Tabular data only 

are provided for a-carotene, trans P-carotene, P-cryptoxanthin, lutein, lycopene, retinyl palmitate, 

y-tocopherol and zeaxanthin. 

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

the past three years. The mean relative standard deviation (RSD of retinol for Core laboratories 

(laboratories that have been involved in the QA program for more than two years) has averaged 

about 11 % over the past three years with a range of 8.5-13.2%. The mean RSD for the New 

laboratories (program participants for less than two years) during the same period of studies is 

approximately 20%. 

The mean RSD of a-tocopherol for Core laboratories has averaged 9.8% with a range of 8.6-

,~ 12.0% over the past three years. During the same period, New laboratory RSD values have 

\_____ averaged about 30% with a range of approximately 7-55%. 

The mean RSD for P-carotene of Core laboratories (using data for all sera with concentrations 

higher than 200 ng/mL) averaged 21 % over the past nine Round Robin studies. The New 

laboratory mean RSD during this period was approximately 34%. These different levels of 

performance (for Core vs New Labs) document the impact of the QA program in improving the 

Quality of Fat-Soluble Vitamins measurements. 

Tables 2 and 3 provide a listing of data submitted in Round Robins XXVII and XXVIII. A 

detailed discussion of data provided in these studies were distributed earlier. The "Core Lab 

Trimmed Averages" were used as Assigned Values for these samples. In Round Robin XXVll, 

the mean RSD for retinol of the Trimmed Core laboratories was approximately 6%, 7% for atocopherol, and 14% for P-carotene. The mean RSD for retinol and a-tocopherol of the 

Trimmed Core laboratories in Round Robin XXVIII was about 6% and approximately 14% for 

P-carotene. 

Tables 4-20 provide a summary of data submitted for the most recent Round Robin (XXIX). 

Five serum samples (186-190) were distributed for analysis in Round Robin XXIX. Serum 189 

and 190 were liquid-frozen samples; the remaining samples were lyophilized. All of these 

samples were distributed in previous Round Robin exercises. Agreement between values 

determined in Round Robin XXIX and previous Round Robins is shown graphically in Section 

( 2C. 

J3
 
( 

c 

( 

In Round Robin XXIX, forty-five laboratories submitted data for retinol: 23 Core labs and 22 

New labs (6 with two-year participation, 5 with one- to two-year participation, and 11 

participating for less than one year). The mean RSD for retinol of the Core laboratories is 

approximately 13% and about 18% for the New laboratories. The mean RSD of the Trimmed 

Core labs for retinol is 4.9%. 

Forty-six laboratories submitted data for a-tocopherol in Round Robin XXIX: 26 Core labs and 

20 New labs (6 two-year participants, 5 one- to two-year participants, and 9 less than one-year 

participants). The mean RSD for the Core laboratories is about 12%, while the Trimmed Core 

mean RSD is 6.2%. The mean RSD for the two-year participants is about 14%, 55% for the oneto two-year participants, and 34% for those laboratories that have participated for less than one 

year. 

Thirty-six laboratories submitted data for ~-carotene in Round Robin XXIX: 20 Core labs and 

16 New labs (5 two-year participants, 4 one- to two-year participants, and 7 less than one-year 

participants. The mean RSD for ~-carotene of the Trimmed Core laboratories is approximately 

12%. The mean RSD of the two-year and one- to two-year participants is 34.5% and 67 .3%, 

respectively. The mean RSD of the laboratories with less than one year participation is 

approximately 41 %. 

Tables 7-20 provide summaries of data submitted for other fat-soluble vitamins and carotenoid 

compounds in Round Robin XXIX. We will continue to improve the measurement quality of 

retinyl palmitate and additional carotenoid compounds. 

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-practice. 

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, 

we suggest that they contact Mrs. Jeanice Brown Thomas at 301/975-3120 or Dr. Kathy Sharpless 

at 301/975-3121 for consultation. We are willing to provide in-house 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 1994" program. An invoice to that effect will 

be mailed to those laboratories. 

The 1994 QA Program will consist of three round robin exercises for the analysis of fat-soluble 

vitamins and carotenoid compounds in serum, two studies for the analysis of ascorbic acid in 

serum, and one exercise for the analysis of fat-soluble vitamins and carotenoid compounds in 

food. 

J4
 
I 

\ 

(_ 

The first set of samples for the fat-soluble vitamins in serum analysis will be distributed the week 

of January 17 with results due March 19; written feed back will be provided to labs by April 25. 

The second set of samples will be shipped the week of April 25 with results due by June 14 and 

feedback to labs by July 25. The third set of samples will be shipped the week of July 25. 

Results will be due by August 30 so that we can discuss all three exercises at the QA Workshop. 

The actual date has not been set yet. Feedback will also be provided to those who are not able 

to attend the workshop. 

The round robin study concerning the analysis of fat-soluble vitamins and carotenoid compounds 

in food will also be scheduled in April to coincide with the second fat-soluble vitamins in serum 

round robin study. The coordinator of this exercise is Dr. Kathy Sharpless (301/975-3121). 

The first set of samples for the analysis of ascorbic acid in serum will be distributed in January 

or February. The second set will be distributed in June. This round robin study is being 

coordinated by Dr. Sam Margolis (301/975-3137). 

J5
 
(1 ( ''i 

.• 1 

..... . 

Table la 

ROUND ROBIN lCXI ROUND ROBIN )()(M ROUND ROBIN XXIU 

RETINOL RETINOI. RETINOL 

SERUM ii SERUM ii SERUM 11 SERUM 11 SERUM 11 SERUM ii SERUM ii • SERUM 11 SERUM ii SERUM ii SERUM ii 

144 145 148 147 148 149 150 155 156 157 159 

GRAl'.01341 0.1113 0504 0.538 0.278 GRAt-1>(44) 0.210 0.510 0680 GRAN>(44) O."I 0401 0.980 0496 

RSC 18.1 15.11 19.1 23.1 RSC 42.8 33.0 312 RSC 15.0 14.8 15.8 17.8 

CORE (30) 01113 0.4114 0.520 0 211 . CORE (31) 0.1117 D.1508 0.682 CXH(30I 0.531 0.402 1.004 0508 

RSD ID Ill 10.I tl.0 RSD 11.5 II Ill RSD 122 102 130 99 

NEW NEW(l2) 0245 0521 0729 NEW(l4) 0514 0398 0.925 0475 RSO RSD 85.7 81.7 684 RSD 205 224 208 292 

ASSIGNED 0958 0490 0.514 0262 ASSIGNED D.1111 0489 0659 ASSIGNED 0536 0405 1010 0506 

RSC 8.5 78 10.0 1.7 RSC 5.4 5.0 71 RSO 4.8 8.5 54 59 

PREVIOl.6 0.1121 0.485 0.515 0.259 PREV10US PRElllOlS 0.489 

DATE IAll 1,g) 5,gi 1,g) DATE DATE 1/91 

a-TOCa>HERCL a-TOCa>HERCL a-TOCa>HERCt. 

GRAND(35) 10.7 6118 5.64 4.88 GRAN0(44) 4.80 10.52 11140 GRAND(44) 7.52 1001 6.30 1051 

RSO 11.0 112 11.3 12.8 RSO 21.4 27.3 27.2 RSC 12.9 IU 14.0 150 

CORE (33) 108 692 669 503 CORE (34) 4.79 1035 1632 CORE (32) 744 989 630 1069 

RSO 8.0 82 11.4 12.5 RSO 10.5 911 90 RSC 8.3 I I.I 8.8 8.4 

NEW NEW(10) 4.82 11.07 II 78 NEW(12) 7.71 1027 6.30 10.05 

RSD ASD 54.0 537 558 RSD II ao u .. ti. 

ASSIGNED 10.7 6111 1159 488 ASSIGNED 480 10.50 11159 ASSIGNED 765 1016 628 10.SO 

RSD 60 35 117 14 ASD 13 30 31 ASD 411 5.4 54 39 

PREVIOUS 105 1168 665 483 PREVIOUS PREVIOUS 

DATE 1/118 11111 5JllO t/llO DATE CATE 10.5 

1/91 

b-CAAOTENE b-CAROl'ENE b-CAROTENE 

GRAND(24) 0836 1144 0236 0.450 GRAND(33) 0275 OJl!M 2.362 ORAND(32) 0378 0.123 0.139 0.898 

RSC 30.5 27.8 85.8 27.3 RSO 34.8 17.5 18.0 RSC 52.7 28.11 189 38.0 

CORE (21) 0.887 1.151 0.211 0.457 CORE (23) 0.292 0.891 2.339 CORE C201 0.348 0.804 0.088 0.856 

RSD 26.5 29.4 39.I 28.3 RSD 34.8 1311 14.4 RSD 24.8 18.9 343 209 

NEW NEW(IO) 0238 0.898 2415 NEW(12) 0426 0854 0221 0965 RSD RSD 31.1 252 249 RSD 712 421 203 492 

ASSIGNED 0848 I 089 0195 0422 ASSIGNED 0260 0890 2 3311 ASSIGNED 0.371 0822 0091 0879 

RSO 4.8 82 8.8 1.4 RSC 22.7 II.I 1.3 RSO 13.8 15.I 19.3 12.4 

PREV10US 0.798 1.034 0.1811 0.408 PREVIOl.6 PRElllOlS 0.890 

DATE IAll 1,g) 5,gi 1,g) DATE DATE ..S/91 

J6
 
n 

ROUNO ROBIN lCXIV RETINQ. 

SAMf\.E ti SAMf\.E ti SAMPLE ti SAMf'lE ti 

160 161 182 183 

1002 0681 0.281 0.387 GRANO 1281 

RSO 242 150 18.2 13.8 ASO 

CORE 1291 I 012 08711 0293 0388 COOE 12:11 

RSD 112 17 70 71 RSD 

NEW(t3) I 0&9 0703 0282 0393 NEW (5) 

RSD 302 238 327 21.4 RSD 

ASSIGNED I 019 0&73 0293 0383 ASSIGNED 

RSO 44 1111 70 117 RSO 

PREVIOl.6 1 DID D659 0291 03811 PREVIOl..6 

DATE 08i!ll 05,91 OSSO DIAlll DATE 

a - TOCOPHEIQ. 

G'IAN0(41) 1123 1595 461 5.114 GRANO(JO) 

ASO 1511 1011 13.1 12.1 RSO 

COOE (JO) 624 1612 463 566 COOE (24) 

RSO 14.o 7.4 II.II 1.2 ASO 

NEW(lll 1121 1541 4.411 U5 NEWl&I 

RSD 210 178 320 2011 RSD 

ASSIGNED 839 1595 461 566 ASSIGNED 

RSD 51 55 87 10 RSD 

PREVIOUS 528 1651 462 584 PREVIOUS 

DATE 0&91 05'91 05AIO 01.U DATE 

b-CAROTENE 

G'IAND (33) OtOO 2205 tDt8 D 1113 GIAN0(27) 

ASO 51.2 32.9 22.0 21.5 ASO 

CORE 1211 0.088 2.223 1.092 0.11$ CORE 1211 

RSD 5111 294 179 129 RSD 

NEW (12) 0.109 2.17 0.881 0.158 NEWiii 

RSD 53.1 43.D 22.1 33.3 RSO 

ASSIGNED 0090 2212 1073 01115 ASSIGNED 

RSO 11 .0 Ill 111 12.11 RSC 

PREVIOUS 009.I 2338 t 145 0202 PREVIOUS 

DATE 08.91 05,91 05i90 01.U DATE 

n ·. 

Table lb 

ROUNO ROBIN lOCV RETINQ. 

SAMf'LE ti SAMf'LE ti SAMf\.E ti SAMPLE ti 

184 Ul5 188 187 

1.074 0:-.411 0202 GRANl(331 10.2 11.5 12.2 20.2 ASO 1.071 0.185 0.539 0187 C00E 1281 

102 122 115 149 RSD 

1037 0866 0560 0224 NEW (7) 

t3t 132 110 352 RSD 

I 085 0172 0525 Dl!M ASSIGNED 

112 II.I 4 I 13 RSC 

1.022 0.841 0.515 PAEVIOl.6 

07Al8 OUIO 05.SO D5St DATE 

a-TOOOPHEIQ. 

U'D 112 411 564 QRAN0(35) 

13.3 ID 13.1 12.I RSO 

145 151 463 566 COOE 1281 

81 ... II.I 12 RSD 

10.111 10.88 1.60 551 NEW j7) 244 111 222 211 RSD 

138 159 836 466 ASSIGNED 

68 1511 12 .. RSD 

1139 11112 155 4.lo PREVIOUS 

07.U OIAIO Cl5.4IO 05Al1 OAT& 

b- CAROrENE 

t.DB7 2D38 0221 0300 QRAN0(30) 

35.7 25.2 113 119.7 RSO 

0 91111 1.1199 0.172 0.2&4 CCIAE1231 

173 13.5 tll 1115 RSD 

1.405 2.247 0.415 0.435 NEW (71 

622 442 131 101 RSD 

1023 2030 0 .1111 0256 ASSIGNED 

12.9 11.7 14.D 1.2 RSO 

1027 U76 OIB9 PREVIOl.S 

01Alll OIAIC> D5AIO D5ill1 DATE 

ROUNO ROBIN lOCVI RETINQ. 

\ , ' ' . 

SAMPLE ti SAMPLE ti SAMf\.E ii SAMf\.E ti SAMf\.E ti 

188 169 170 171 172 

0.:-.48 0644 0669 0:-.47 0&10 

1011 10.7 117 7.0 81 

0.:-.48 0.844 0668 0:-.47 0667 

1U t2.1 88 17 67 

0559 0648 0680 0548 0680 71 47 72 87 75 

0548 0639 0657 0538 0662 

411 73 52 49 58 

0.553 0.827 

ID.SO 1DSO 

a-Toca>HEROL 

1D.51 112 1125 496 81B 

II.II u 10.1 11.5 u 

t0.41 115 821 4.113 813 

8.7 •• 10.3 12.1 17 

1124 1.70 11311 508 8311 118 88 17 15 12 

10.33 1183 523 503 513 

411 111 Ill 17 118 

1041 1185 

10AIO 1CIAIO 

b-CAllOfENE 

U62 0439 0621 04CJD Ofi09 

17.1 22.2 17.5 11111 18.4 

1.110 0 .447 0.1142 0411 0.823 

165 23.9 17.4 141 153 

1.5111 0.415 0.553 0.348 0 5114 .

23.9 14.5 12.4 173 193 

1718 0 .450 OIU7 0416 05118 

1.0 14.3 II.II 14.11 11.9 

U111 0 441 .

llWO 1DAIO 

J7
 
Round Robin XXVll 

Retlnol 

Sample # Sample # Sample # Sample # Sample # 

173 114 175 176 1n 

Grand (38) 0.503 

RSD 11.1 

Core (27) 0.496 

RSD 10.5 

Assigned 0.502 

RSO 5.1 

Previous Date 

0.489 

5191 

0.506 

8191 

Grand (34) 10.53 

RSD 9.7 

Core (25) 10.55 

RSD 7.1 

Assigned 10.69 

RSO 5.5 

Previous Date 

10.50 

5191 

10.42 

8191 

Grand (33) 0.936 

RSD 23.9 

Core (24) 0.931 

RSD 15.4 

Assigned 0.909 

RSD 6.8 

Previous 

Dale 

0.890 

5191 

0.879 

8191 

0.539 

13.8 

0.530 

13.5 

0.542 

5.7 

0.536 

8191 

7.37 

12.6 

7.35 

11.1 

7.55 

4.3 

7.55 

8191 

0.416 

53.9 

0.399 

41.1 

0.368 

16.1 

0.371 

8191 

0.405 

11.1 

Q.400 

11 .2 

0.394 

6.2 

0.405 

8191 

0.545 

11.5 

0.543 

11.0 

0.541 

6.2 

0.538 

8192 

a-Tocopherol 

9.93 9.7 9.98 

7.6 

10.12 

6.0 

10.16 

8191 

Ji-Carotene 

0.875 

35.6 

0.843 

21 .2 

0.844 

15.2 

0.822 

8191 

4.87 

12.6 

4.82 

12.8 

4.n 

11.9 

5.03 

8192 

0.435 

38.8 

0.430 

32.9 

0.414 

15.1 

0.416 

8192 

0.673 

16.5 

0.673 

16.2 

0.671 

6.3 

0.659 

5191 

0.673 

1192 

15.74 

8.5 

15.74 

8.5 

15.70 

6.6 

16.59 

5191 

15.95 

1192 

2.37 

18.1 

2.37 

18.1 

2.37 

18.1 

2.34 

5191 

2.21 

1192 

!"1 

Table le 

Round Robin XXVlll 

Retlnol 

Sample # Sample # Sample # Sample # Sample # 

181 182 183 184 185 

Grand (39) 0.494 

RSD 13.6 

Core (23) 0.484 

RSD 10.7 

Assigned 0.472 

RSD 7.8 

Grand (39) 6.86 

RSD 16.6 

Core (25) 7.oo 

RSO 8.0 

Assigned 7.03 

RSD 5.6 

Grand (29) 0.119 

RSD 100.4 

Core (19) 0.087 

RSD 26.1 

Assigned 0.081 

RSD 18.0 

0.543 

16.9 

0.540 

8.5 

0.531 

6.8 

5.38 

16.0 

5.41 

7.5 

5.36 

5.8 

0.441 

22.0 

0.430 

15.2 

0.420 

12.4 

0.558 

17.0 

0.554 

8.9 

0.545 

4.7 

0.362 

19.7 

0.353 

10.2 

0.344 

5.9 

a-Tocopherol 

10.99 14.8 

11.24 

7.0 

11 .31 

6.3 

Ji-Carotene 

0.372 

20.7 

0.371 

16.6 

0.364 

15.0 

4.41 

24.8 

4.44 

14.7 

4.22 

6.1 

0.352 

17.7 

0.362 

16.6 

0.354 

14.5 

0.555 

14.1 

0.545 

11 .2 

0.525 

6.2 

5.38 

18.4 

5.50 

9.8 

5.42 

5.5 

0.436 

20.8 

0.448 

20.8 

0.428 

11.9 

Grand (45) 

RSO 

Core (23) 

RSO 

Assigned 

RSO 

Previous Date 

Grand (46) 

RSD 

Core (26) 

RSO 

Assigned 

RSO 

Previous Date 

Grand (36) 

RSD 

Core (20) 

RSO 

Assigned 

RSD Previous Date 

Round Robin XXIX 

Retlnol 

Sample # Sample # Sample # Sample # Sample # 

186 188 189 

0.222 

21 .8 

0.233 

20.7 

0.227 

7.6 

0.226 0.221 

3.54 

23.8 

3.72 

10.1 

3.68 

4.7 

3.74 

3.71 

0.933 

42.4 

0.899 

17.1 

0.862 

11.8 

0.974 

0.864 

0.505 

20.9 

0.534 

19.3 

0.487 

3.8 

0.485 

6.55 

24.4 

6.98 

15.9 

6.78 

4.6 

6.68 

6.91 

1.08 

49.5 

1.02 

18.8 

1.04 15.8 1.04 1.09 

0.722 

15.0 

0.745 

8.7 

0.734 

4.4 

0.738 0.729 

0.625 

13.7 

0.641 

7.5 

0.636 

4.1 

0.627 0.639 

a-Tocopherol 

11.16 

22.4 

11 .70 

10.3 

11 .31 

7.8 

11 .88 

11 .56 

Ji-Carotene 

0.503 

41 .1 

0.484 

18.0 

0.782 

10.8 

0.524 0.523 

9.25 

22.5 

9.7 

12.4 

9.47 

6.2 

9.65 9.83 

0.435 

38.6 

0.424 

19.0 

0.438 

13.0 

0.441 0.456 

0.540 

15.1 

0.550 

9.9 

0.542 

4.5 

0.553 0.546 

10.11 

22.6 

10.60 

11.2 

10.27 

7.7 

10.46 

10.33 

1.65 

43.4 

1.83 

14.4 

1.58 

9.1 

1.62 

1.72 

J8
 






J1

5
J1

6
J1

7
 

 

Appendix K. Representative “Individualized Report” for RR29 

Each participant in RR29 received graphical summaries of their own measurement 

performance for total retinol, α-tocopherol, and/or total β-carotene. In RR29, 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 7/93. 

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

just the sera distributed in RR29. 

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

K1
 
(\ 

Percent Bias 

() '· , 

Laboratory FSV-By_ 

Retinol 

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

10 - - . - . . - .. - . - - - . - .. - .... - .. - - . - .... _ ........ - - ..... - . - . - . .. - - . - - - - - . - - .. - . . . . . - . - -

0 L..1tii'.it.tUkiF.iHt.tHHM ut.tUUhiHHnHHHHMNl-.li·il .IHMMMl:Jl·.IMMMUUUMfl f·tt-lt·it·t Hl-11-1 M .... l:'ll·i UHi 1M f·ii ·IMl ·I I ·! nttt:t Jttt 11Litt UHffl .111 1.tr .t' 11 II, 

-10 .. - - - - - - - . . . . . . . . . . . - .. u - .. . ... .... .. . . . .... . .. .. . ....... .. . . 

-30 I . 

-20 

·1 1· . . 

.. i:: •• - • •••. ••.• . • .•. • . .. •.. '1 •• •••• • •• • •.• • • • • • ••. • • •••• • ..• - .•• . . 

8/92 1/93 4/93 7/93 

o/o Bias from Assigned Values 

,,--, 

/ 

K2
 
r--.. 

30 

20 

10 

Percent Bias 

17) 

Laboratory FSV-BY 

Alpha-Tocopherol 

: : 

. . . . •· : •: • I 

- rom HHW H HH ... a _ U LJ UHU , ' . . • • • . . • • • • • • • B 0 I H -n UUUHHUU U-UHHBHH "HMM nu UH • ll IJ 0 '111"-u, 0111 

-10 

-20 

-30 1 /93 4/93 7 /93 

% Bias from Assigned ·Values 

(""} 

K3
 
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ca 

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~ 

i;;:;= = · = · 

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.. · .. ·.·.· .. ·.':] 

·"""··-·.'.':':'.":') 

~ 

18.L .. 1 

s==1 

c::b= 

t;J 

0 

I 

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~ 

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N 

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ca 

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'#. 

K4
 
(\ 

% Bias 

Laboratory ,FSV-BY 

Blind Duplicate Performance 

Retinal 

30-.. 

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

10 .............. .. ...................... - ............ .. .................... .. 

OJ t :-:·:·:ii.:.:.:-: .. 11 ... :.:.:-:I 

-10 : : ..: : -. - . - - - - .. -. .. - .. . - - .. - - - .. 

-20· ---------. ------. -----. -------------------. . -. .. -------. . -.. . ---. -.. -

-30 149 159 173 155 174 156 175 171 176 150 161 177 162 185 130 142 186 121 145 187 133 140 188 139 169 189 138 166 190 

Serum I 

5/91 8/91 1/93 8/91 1/93 8/91 1/93 8/92 1/93 5/91 1/92 1/93 4/93 4/93 5/90 9/90 7/93 1190 1191 7/93 5/90 9190 7/93 9190 8192 7/93 9/90 8192 7193 

,- ' I \ 

K5
 
(', 

o/o Bias 

I 

Laboratory iFSV-BY 

Blind Duplicate Performance 

Alpha-Tocopherol 

20 r · · · · · · · · · · · · · - - - - - - · · · - - - · · - - - - · - · - - - - · - - - · · - - - - - - - - - - - - - ........... . 

. . ·.·. 

1 0 t .. - - ; .. -. - - - -. - - ' - ....... - - . - ... - .... - - -· ... - - . - - - - - - - .... - .. - ...... . 

0 I I . . I · J -·.·· 1· : · :· . c=:i• ·. I ... I II II I I I I I I II I I I I I I I I I I · - 1 I . · C:::::S I Ii I t:::::!Ji I I ii I I I I I I I 

-10 I· - - - -:_ - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - · - - - - - - - - - - - - - - - - - - - - - - - - - - - - -

-20 1 - - - - - .. - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - . - - - - - - - - . - - - . - ..... - - . . - - -

-30 130 142 186 121 145 187 133 140 188 139 169 189 138 168 190 

Serum I 

5/91 8/91 1/93 8/91 1/93 8/91 1/93 8/92 1/93 5/91 1/92 1/93 4/93 4/93 5/90 9/90 7/93 1/90 1/91 7/93 5/90 9/90 7/93 9190 8/92 7193 9190 8192 7/93 

'.) 

K6
 
' 

% Bias 

(\ 

Laboratory FSV-BY 

Blind Duplicate Performance 

Total Beta-Carotene 

20 ... .; ....... .. · ...... .; .... ..; ... · ................ . ............ .... - .. - - .......... .. .......... - - .... .. 

10 

Q I ·· mli!!jrqi l"'lrqi·. ,·• rqim [j!ijrqi •• mpqm m,,,,;, · ·. Wh'lllma -=1"'1 lk,, 

-10 .. .. -· .. ·- - - - - .. - - ·- - : - - - .. - - - -. - - - - - - - - - - . - - - - - - - - - . - - - - - - . - - -

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

-30 149 159 173 155 174 156 175 171 176 150 161 177 182 185 130 142 186 121 145 187 133 140 188 139 169 189 138 168 190 

Serum I 

519181911193 81911193 8/911/93 8/921/93 5/9111921/93 4/934/93 5/9091907193 1/901/917193 51909/907/93 9/9081927/93 9/908/927/93 

('\ 

K7
 
 

 

 

 

Appendix L. Updated “All-Lab Report” for RR29 

The following six pages are an updated version of an “All-Lab” report for RR29. This 

report has three parts: 

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

participants and NIST analysts. 

•	 page 5 lists values for all analytes reported by only once. This page also provides 

a legend for pages 1 to 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 RR29 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 RR29. 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 NISTa and NISTb in this updated All-Lab report are 

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

L1
 
 

Round Robin XXIX Laboratory Results 

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

Lab 186 187 188 189 190 

FSV-BA 0.238 0.494 0.749 0.635 0.548 

FSV-BD 0.250 0.517 0.776 0.634 0.528 

FSV-BE 0.210 0.468 0.730 0.633 0.542 

FSV-BF 0.230 0.489 0.749 0.642 0.551 

FSV-BG 0.213 0.483 0.723 0.635 0.431 

FSV-BH 0.206 0.467 0.674 0.595 0.525 

FSV-BI 0.215 0.463 0.732 0.594 0.508 

FSV-BJ 0.240 0.505 0.764 0.640 0.558 

FSV-BK 0.201 0.455 0.657 0.710 0.626 

FSV-BL 0.428 0.894 0.716 0.682 0.563 

FSV-BM 0.186 na 0.707 0.636 0.558 

FSV-BN 0.216 0.517 0.796 0.620 0.595 

FSV-BO 0.161 0.363 0.536 0.553 0.519 

FSV-BP 0.238 0.498 0.724 0.616 0.521 

FSV-BQ 0.201 0.485 0.746 0.588 0.526 

FSV-BR 0.227 0.512 0.755 0.648 0.530 

FSV-BT 0.215 0.458 0.767 0.721 0.587 

FSV-BY 0.206 0.478 0.739 0.647 0.559 

FSV-BZ 

FSV-CA 0.243 0.493 0.697 0.563 0.514 

FSV-CB 0.313 0.493 0.777 0.626 0.561 

FSV-CG 0.079 0.150 0.221 0.182 0.165 

FSV-CH 0.242 0.668 0.967 0.788 0.689 

FSV-CJ 0.260 0.598 0.845 0.745 0.679 

FSV-CK 0.212 0.685 0.713 0.602 0.550 

FSV-CM 

FSV-CO 0.218 0.466 0.726 0.592 0.510 

FSV-CP 

FSV-CQ 0.250 0.520 0.780 0.670 0.580 

FSV-CR 0.238 0.515 0.753 0.630 0.547 

FSV-CT 0.184 0.687 0.830 0.706 0.613 

FSV-CU 0.238 0.506 0.767 0.652 0.551 

FSV-CV 0.212 0.483 0.720 0.630 0.550 

FSV-CX 0.250 0.550 0.830 0.660 0.520 

FSV-CY 0.219 0.499 0.728 0.648 0.499 

FSV-DJ 0.210 0.490 0.510 0.710 0.610 

FSV-DM 0.238 0.498 0.797 0.628 0.521 

FSV-DS 0.304 0.492 0.750 0.625 0.602 

FSV-DX 0.212 0.448 0.710 0.571 0.477 

FSV-EA 0.264 0.501 0.677 0.656 0.604 

FSV-EB 0.233 0.485 0.684 0.656 0.561 

FSV-EC 0.170 0.336 0.570 0.460 0.377 

FSV-EI 0.196 0.469 0.621 0.619 0.496 

FSV-EJ 0.154 0.458 0.645 0.678 0.585 

FSV-EK 0.201 0.553 0.833 0.673 0.582 

FSV-EN 0.188 0.451 0.734 0.586 0.502 

FSV-EX 0.200 0.500 0.720 0.630 0.550 

FSV-FC 0.230 0.488 0.721 0.614 0.690 

FSV-FF 0.228 0.488 0.746 0.634 0.542 

186 187 188 189 190 

nd 0.052 0.015 0.087 0.227 

0.055 0.236 

nd nd nd 0.062 0.168 

nd nd nd 0.092 0.295 

nd nd nd 0.084 0.276 

0.163 nd 0.020 0.066 0.279 

nd nd nd 0.069 0.276 

nd nd nd 0.059 0.183 

0.026 0.059 0.066 0.073 0.183 

186 187 188 189 190 

3.79 6.66 11.41 9.60 9.97 

3.50 6.40 10.40 8.90 9.50 

4.36 8.20 13.53 12.51 13.55 

3.74 6.83 11.80 10.27 10.85 

3.23 6.24 10.81 9.56 10.64 

3.83 6.69 12.62 9.56 10.26 

3.64 6.58 11.64 9.60 10.16 

3.87 7.24 11.26 9.81 10.64 

3.40 6.85 11.11 9.69 10.41 

3.88 7.00 12.22 9.44 10.16 

3.60 na 11.50 9.70 10.40 

5.02 7.17 13.47 10.02 12.86 

2.88 5.22 8.78 9.31 10.65 

2.75 6.60 13.70 9.91 10.03 

3.86 6.24 11.68 9.33 10.01 

4.13 7.54 11.47 9.34 10.36 

3.73 6.70 11.53 9.47 10.47 

3.16 4.50 9.74 6.69 8.90 

3.58 6.56 10.93 8.40 9.43 

2.60 5.70 13.10 10.10 10.40 

0.46 0.84 1.34 1.12 1.24 

4.25 10.10 13.90 11.20 12.40 

3.67 7.12 11.61 9.79 11.50 

3.38 9.29 11.24 9.73 10.12 

3.67 6.84 12.19 9.53 10.18 

3.57 6.53 11.58 9.44 10.11 

3.10 5.73 9.97 8.32 8.85 

3.86 7.07 12.60 10.06 11.28 

3.85 6.63 11.68 9.03 9.74 

3.83 6.94 10.52 8.38 9.13 

3.49 5.95 10.87 9.03 10.01 

3.48 6.37 11.90 9.23 9.40 

4.10 6.80 10.60 9.40 10.50 

3.94 6.87 11.77 8.50 10.27 

4.20 7.50 13.20 11.70 12.50 

4.84 8.73 15.19 12.27 13.34 

4.07 7.01 11.98 9.47 10.17 

4.17 6.48 10.13 9.16 9.16 

3.47 6.12 10.80 9.90 10.00 

3.77 6.92 10.29 10.26 11.58 

0.13 0.22 0.43 0.36 0.36 

2.89 5.88 10.41 8.86 9.52 

3.91 7.41 12.13 11.35 11.70 

3.71 6.80 12.20 9.56 10.07 

2.95 6.37 10.65 8.10 8.64 

3.66 7.31 11.91 10.43 11.16 

3.40 6.32 10.75 9.43 12.55 

186 187 188 189 190 

0.837 1.104 2.40 2.41 1.50 

0.818 1.102 2.486 2.481 1.543 

0.940 1.020 2.520 2.640 1.460 

0.770 0.960 2.34 2.24 1.37 

0.780 1.020 2.390 2.360 1.430 

0.826 0.891 2.47 2.37 1.46 

0.815 0.997 2.40 2.35 1.47 

0.739 1.108 2.302 2.301 1.482 

0.750 0.690 2.15 1.87 1.84 

0.100 0.160 0.32 0.31 0.21 

0.602 1.070 2.48 2.31 1.49 

0.520 1.000 1.75 1.75 1.03 

0.775 1.230 2.30 2.35 1.53 

0.930 1.100 2.50 2.50 1.55 

0.630 0.830 2.26 2.50 1.39 

0.545 0.774 2.42 2.53 1.49 

nd 1.229 2.73 2.69 1.66 

1.030 1.050 2.69 2.16 1.49 

0.710 0.900 2.24 2.26 1.75 

n 46 45 46 46 46 

Min 0.079 0.150 0.221 0.182 0.165 

Mean 0.223 0.500 0.720 0.627 0.544 

Max 0.428 0.894 0.967 0.788 0.690 

SD 0.048 0.102 0.108 0.086 0.081 

CV 22 20 15 14 15 

2 2 3 9 9 

0.026 0.052 0.015 0.055 0.168 

0.095 0.056 0.034 0.072 0.236 

0.163 0.059 0.066 0.092 0.295 

0.097 0.005 0.028 0.013 0.049 

103 9 84 18 21 

47 46 47 47 47 

0.13 0.22 0.43 0.36 0.36 

3.54 6.55 11.16 9.25 10.11 

5.02 10.10 15.19 12.51 13.55 

0.84 1.60 2.50 2.08 2.29 

24 24 22 22 23 

18 19 

0.100 0.160 

0.729 0.960 

1.030 1.230 

0.206 0.239 

28 25 

19 

0.32 

2.27 

2.73 

0.52 

23 

19 

0.31 

2.23 

2.69 

0.52 

23 

19 

0.21 

1.43 

1.84 

0.34 

24 

NISTa 

NISTb 

0.225 0.501 0.704 0.610 0.535 

0.203 0.462 0.695 0.589 0.510 nd nd nd 0.067 0.246 

3.56 

3.67 

6.55 11.41 9.34 10.08 

6.59 11.30 10.00 10.70 

0.630 0.850 

0.730 0.940 

2.23 

2.32 

2.04 

2.33 

1.25 

1.45 

Median 0.217 0.492 0.731 0.634 0.550 

eSD 0.031 0.034 0.050 0.033 0.045 

eCV 14 7 7 5 8 

0.069 0.236 

0.015 0.064 

21 27 

3.67 

0.36 

10 

6.69 11.53 

0.56 1.07 

8 9 

9.53 10.18 

0.56 0.70 

6 7 

0.773 1.020 

0.094 0.125 

12 12 

2.40 

0.15 

6 

2.35 

0.19 

8 

1.49 

0.08 

5 

L2
 

All Lab Report Page 1 / 6 
Round Robin XXIX Laboratory Results 

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

Lab 186 187 188 189 190 

FSV-BA 0.937 1.082 0.530 0.482 1.732 

FSV-BD 

FSV-BE 1.118 1.364 0.618 0.503 1.953 

FSV-BF 1.349 1.355 0.642 0.506 2.118 

FSV-BG 0.800 1.070 0.408 0.533 1.660 

FSV-BH 0.977 1.124 0.537 0.445 1.686 

FSV-BI 0.886 1.034 0.492 0.424 1.513 

FSV-BJ 0.963 1.090 0.558 0.485 1.820 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 1.099 1.316 0.565 0.495 1.795 

FSV-BO 0.984 1.134 0.489 0.334 1.794 

FSV-BP 0.378 0.984 0.466 0.393 1.342 

FSV-BQ 0.960 0.967 0.470 0.404 1.321 

FSV-BR 

FSV-BT 1.020 1.135 0.547 0.502 1.750 

FSV-BY 0.958 1.078 0.533 0.449 1.689 

FSV-BZ 0.920 0.950 0.470 0.400 1.520 

FSV-CA 

FSV-CB >0.685 >0.679 >0.344 >0.282 >1.256 

FSV-CG 0.180 0.227 0.115 0.099 0.403 

FSV-CH 0.786 1.050 0.462 0.467 1.400 

FSV-CJ 0.706 0.806 0.403 0.356 1.351 

FSV-CK 0.854 0.569 0.424 0.370 1.320 

FSV-CM 

FSV-CO 0.933 1.044 0.529 0.443 1.659 

FSV-CP 0.801 0.914 0.456 0.382 1.463 

FSV-CQ 0.704 0.850 0.243 0.174 1.546 

FSV-CR 

FSV-CT 1.111 1.297 0.494 0.408 1.726 

FSV-CU 0.764 0.851 0.504 0.431 1.526 

FSV-CV 0.985 0.985 0.520 0.420 1.570 

FSV-CX 0.870 1.040 0.520 0.420 0.170 

FSV-CY 0.916 1.200 0.485 0.440 2.070 

FSV-DJ 

FSV-DM 0.897 1.074 0.455 0.362 1.606 

FSV-DS 0.971 1.062 0.539 0.426 1.699 

FSV-DX 0.754 0.439 0.217 0.304 1.032 

FSV-EA 0.757 0.842 0.380 0.359 1.364 

FSV-EB 0.968 1.058 0.498 0.486 1.720 

FSV-EC 2.869 3.825 1.533 1.247 5.095 

FSV-EI 0.447 0.523 0.288 0.268 1.126 

FSV-EJ 0.688 0.733 0.393 0.330 1.230 

FSV-EK 0.913 0.990 0.484 0.390 1.717 

FSV-EN 

FSV-EX 1.070 1.150 0.560 0.490 1.650 

FSV-FC 0.930 1.090 0.505 0.433 1.928 

FSV-FF 1.058 1.352 0.619 0.565 2.111 

186 187 188 189 190 

0.885 1.015 0.499 0.448 1.675 

0.919 1.064 0.509 0.421 1.619 

0.999 1.262 0.627 0.558 1.746 

0.960 1.076 0.525 0.472 1.677 

0.685 0.679 0.344 0.282 1.256 

0.678 0.772 0.383 0.304 1.275 

0.682 0.766 0.445 0.380 1.448 

186 187 188 189 190 

0.052 0.067 0.031 0.034 0.057 

0.058 0.060 0.028 0.024 0.067 

0.121 0.095 0.053 0.066 0.111 

0.060 0.059 0.022 0.030 0.073 

0.028 0.034 0.020 0.052 0.076 

0.082 0.085 0.059 0.051 0.078 

n 

Min 

Mean 

Max 

SD 

CV 

38 

0.180 

0.928 

2.869 

0.386 

42 

38 

0.227 

1.070 

3.825 

0.521 

49 

38 

0.115 

0.499 

1.533 

0.204 

41 

38 

0.099 

0.432 

1.247 

0.164 

38 

38 

0.170 

1.636 

5.095 

0.697 

43 

7 

0.678 

0.830 

0.999 

0.143 

17 

7 

0.679 

0.948 

1.262 

0.212 

22 

7 

0.344 

0.476 

0.627 

0.095 

20 

7 

0.282 

0.409 

0.558 

0.096 

24 

7 

1.256 

1.528 

1.746 

0.202 

13 

6 

0.028 

0.067 

0.121 

0.032 

47 

6 

0.034 

0.067 

0.095 

0.021 

32 

6 

0.020 

0.036 

0.059 

0.016 

46 

6 

0.024 

0.043 

0.066 

0.016 

37 

6 

0.057 

0.077 

0.111 

0.018 

24 

NISTa 

NISTb 

0.962 

0.885 

1.210 

0.934 

0.559 

0.476 

0.495 

0.399 

1.600 

1.500 

0.939 

0.803 

1.160 

0.855 

0.538 

0.443 

0.470 

0.374 

1.540 

1.450 

0.023 

0.082 

0.050 

0.079 

0.021 

0.033 

0.025 

0.025 

0.060 

0.050 

Median 

eSD 

eCV 

0.925 

0.162 

18 

1.054 

0.136 

13 

0.493 

0.062 

13 

0.425 

0.087 

20 

1.655 

0.228 

14 

0.885 

0.169 

19 

1.015 

0.360 

35 

0.499 

0.080 

16 

0.421 

0.076 

18 

1.619 

0.188 

12 

0.059 

0.022 

38 

0.064 

0.019 

30 

0.030 

0.013 

43 

0.043 

0.016 

38 

0.075 

0.008 

11 

L3

All Lab Report Page 2 / 6 
 

Round Robin XXIX Laboratory Results 

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

Lab 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 

FSV-BI 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BT 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CG 

FSV-CH 

FSV-CJ 

FSV-CK 

FSV-CM 

FSV-CO 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CT 

FSV-CU 

FSV-CV 

FSV-CX 

FSV-CY 

FSV-DJ 

FSV-DM 

FSV-DS 

FSV-DX 

FSV-EA 

FSV-EB 

FSV-EC 

FSV-EI 

FSV-EJ 

FSV-EK 

FSV-EN 

FSV-EX 

FSV-FC 

FSV-FF 

186 187 188 189 190 

0.050 0.046 0.019 0.073 0.101 

0.062 0.060 0.022 0.091 0.129 

0.061 0.044 0.025 0.099 0.153 

0.040 0.034 0.021 0.063 0.097 

0.038 0.032 0.019 0.058 0.080 

0.052 0.041 0.024 0.070 0.111 

0.047 0.038 0.027 0.077 0.127 

0.033 0.025 0.014 0.041 0.080 

nd 0.048 0.021 0.077 0.120 

0.037 0.033 0.018 0.070 0.087 

0.045 0.037 0.023 0.060 0.108 

0.038 0.036 nd 0.048 0.081 

0.019 nd nd 0.042 nd 

0.023 0.020 0.015 0.041 0.063 

0.046 0.044 0.036 0.118 0.112 

0.051 0.024 0.025 0.079 0.118 

0.039 0.033 0.019 0.061 0.101 

0.029 0.013 0.008 0.055 0.080 

0.020 0.020 0.020 0.090 0.150 

0.032 nd nd 0.043 0.053 

0.028 0.030 0.014 0.051 0.084 

0.014 0.011 0.008 0.030 0.047 

0.036 0.030 0.024 0.063 0.092 

186 187 188 189 190 

0.095 0.429 0.266 0.466 0.448 

0.098 0.372 0.209 0.353 0.341 

0.082 0.339 0.195 0.319 0.300 

0.091 0.350 0.223 0.375 0.349 

0.102 0.382 0.261 0.432 0.430 

0.054 0.213 0.121 0.216 0.224 

0.122 0.722 0.404 0.570 0.630 

0.082 0.073 0.178 0.311 0.293 

0.120 0.427 0.249 0.404 0.404 

0.090 0.200 0.126 0.185 0.250 

0.021 0.065 0.040 0.065 0.068 

0.005 0.017 0.011 0.017 0.019 

0.112 0.435 0.232 0.428 0.368 

0.098 0.348 0.224 0.362 0.362 

0.158 0.321 0.288 0.491 0.498 

0.088 0.320 0.196 0.332 0.321 

0.117 0.409 0.285 0.405 0.380 

0.080 0.330 0.200 0.370 0.390 

0.060 0.246 0.147 0.236 0.343 

0.034 0.131 0.093 0.152 0.171 

0.217 0.287 0.218 0.300 0.361 

0.078 0.329 0.188 0.323 0.311 

186 187 188 189 190 

0.062 0.226 0.139 0.222 0.219 

0.074 0.339 0.222 0.321 0.333 

0.062 0.119 0.073 0.191 0.164 

186 187 188 189 190 

0.052 0.148 0.053 0.140 0.156 

0.051 0.175 0.056 0.159 0.183 

0.039 0.125 0.037 0.110 0.133 

0.039 0.125 0.041 0.103 0.130 

0.029 0.089 0.022 0.093 0.116 

0.017 0.100 0.044 0.108 0.106 

>0.096 >0.135 >0.046 >0.12 >0.146 

0.042 0.120 0.037 0.098 0.127 

0.024 0.067 0.024 0.061 0.073 

0.003 0.011 0.004 0.010 0.012 

0.048 0.102 0.045 0.102 0.134 

0.093 0.134 0.052 0.129 0.152 

0.034 0.107 0.033 0.100 0.115 

0.020 0.080 0.020 0.080 0.110 

0.021 0.073 0.025 0.064 0.080 

nd 0.208 nd 0.170 0.247 

n 

Min 

Mean 

Max 

SD 

CV 

22 21 20 23 22 

0.014 0.011 0.008 0.030 0.047 

0.038 0.033 0.020 0.065 0.099 

0.062 0.060 0.036 0.118 0.153 

0.013 0.012 0.006 0.021 0.028 

34 36 32 33 28 

22 22 22 22 22 

0.005 0.017 0.011 0.017 0.019 

0.091 0.307 0.198 0.323 0.330 

0.217 0.722 0.404 0.570 0.630 

0.045 0.154 0.087 0.135 0.133 

49 50 44 42 40 

3 3 3 3 3 

0.062 0.119 0.073 0.191 0.164 

0.066 0.228 0.145 0.245 0.239 

0.074 0.339 0.222 0.321 0.333 

0.007 0.110 0.075 0.068 0.086 

10 48 52 28 36 

14 

0.003 

0.037 

0.093 

0.022 

59 

15 

0.011 

0.111 

0.208 

0.047 

42 

14 

0.004 

0.035 

0.056 

0.015 

42 

15 

0.010 

0.102 

0.170 

0.040 

39 

15 

0.012 

0.125 

0.247 

0.052 

42 

NISTa 

NISTb 

0.060 0.037 0.033 0.066 0.115 

0.069 0.056 0.031 0.072 0.130 0.169 0.491 0.300 0.484 0.503 0.066 0.215 0.134 0.202 0.206 0.023 0.067 0.020 0.060 0.074 

Median 

eSD 

eCV 

0.038 0.033 0.021 0.063 0.099 

0.013 0.012 0.005 0.021 0.028 

35 35 24 33 28 

0.091 0.330 0.205 0.343 0.346 

0.025 0.121 0.075 0.110 0.073 

28 37 37 32 21 

0.037 

0.020 

55 

0.107 

0.040 

37 

0.037 

0.019 

50 

0.102 

0.033 

32 

0.127 

0.031 

25 

L4
 

All Lab Report Page 3 / 6 
 

Round Robin XXIX Laboratory Results 

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

Lab 186 187 188 189 190 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BH 0.042 0.136 0.074 0.126 0.140 

FSV-BI 0.043 0.118 0.071 0.117 0.144 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.037 0.136 0.074 0.128 0.156 

FSV-BO 0.059 0.156 0.108 0.216 0.255 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BT >0.056 >0.136 >0.103 >0.168 >0.175 

FSV-BY 0.040 0.111 0.072 0.108 0.133 

FSV-BZ 0.038 0.100 0.060 0.091 0.108 

FSV-CA 

FSV-CB 

FSV-CG 

FSV-CH 

FSV-CJ 

FSV-CK 

FSV-CM 

FSV-CO 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CT 0.047 0.104 0.076 0.099 0.114 

FSV-CU 

FSV-CV 

FSV-CX 0.060 0.090 0.120 0.180 0.230 

FSV-CY 

FSV-DJ 

FSV-DM 

FSV-DS 

FSV-DX 0.036 0.105 0.064 0.097 0.116 

FSV-EA 

FSV-EB 

FSV-EC 

FSV-EI 0.013 0.048 0.027 0.042 0.050 

FSV-EJ 

FSV-EK 0.053 0.207 0.138 0.223 0.267 

FSV-EN 

FSV-EX 

FSV-FC 

FSV-FF 

186 187 188 189 190 

0.024 0.029 0.028 0.025 0.025 

0.023 0.033 0.026 0.044 0.043 

0.021 0.042 0.032 0.053 0.045 

>0.019 >0.027 >0.031 >0.048 >0.048 

0.013 0.031 0.025 0.039 0.045 

0.180 0.410 0.289 0.430 0.536 

0.024 0.038 0.039 0.027 0.024 

0.002 0.017 0.010 0.012 0.020 

186 187 188 189 190 

0.103 0.257 0.153 0.246 0.263 

0.066 0.165 0.102 0.151 0.165 

0.066 0.151 0.097 0.161 0.187 

0.069 0.182 0.117 0.190 0.226 

0.101 0.240 0.196 0.334 0.354 

0.065 0.158 0.102 0.159 0.187 

0.056 0.120 0.119 0.150 0.183 

0.062 0.184 0.117 0.200 0.223 

0.086 0.300 0.150 0.217 0.254 

0.071 0.174 0.110 0.174 0.195 

0.071 0.142 0.115 0.126 0.138 

0.015 0.065 0.037 0.054 0.070 

n 

Min 

Mean 

Max 

SD 

CV 

11 

0.013 

0.043 

0.060 

0.013 

30 

11 

0.048 

0.119 

0.207 

0.041 

34 

11 

0.027 

0.080 

0.138 

0.031 

38 

11 

0.042 

0.130 

0.223 

0.055 

43 

11 

0.050 

0.156 

0.267 

0.067 

43 

7 

0.002 

0.041 

0.180 

0.062 

151 

7 

0.017 

0.086 

0.410 

0.143 

167 

7 

0.010 

0.064 

0.289 

0.100 

155 

7 

0.012 

0.090 

0.430 

0.151 

167 

7 

0.020 

0.105 

0.536 

0.190 

180 

12 

0.015 

0.069 

0.103 

0.023 

33 

12 

0.065 

0.178 

0.300 

0.063 

35 

12 

0.037 

0.118 

0.196 

0.038 

32 

12 

0.054 

0.180 

0.334 

0.068 

38 

12 

0.070 

0.204 

0.354 

0.070 

34 

NISTa 

NISTb 0.040 0.117 0.074 0.115 0.143 0.026 0.045 0.039 0.053 0.055 0.066 0.162 0.113 0.168 0.198 

Median 

eSD 

eCV 

0.042 

0.007 

18 

0.111 

0.031 

28 

0.074 

0.015 

20 

0.117 

0.030 

25 

0.140 

0.039 

28 

0.023 

0.003 

13 

0.033 

0.007 

22 

0.028 

0.006 

21 

0.039 

0.021 

53 

0.043 

0.027 

62 

0.068 

0.007 

10 

0.169 

0.034 

20 

0.116 

0.021 

18 

0.168 

0.041 

24 

0.191 

0.050 

26 

L5

All Lab Report Page 4 / 6 
Round Robin XXIX Laboratory Results 

Analytes Reported By One Laboratory 

Values in μg/mL 

Analyte Code 186 187 188 189 190

δ-Tocopherol NISTb nd 0.109 0.142 0.104 0.076

trans-α-Carotene NISTb 0.048 0.043 0.024 0.068 0.097

trans-β-Cryptoxanthin FSV-BT 0.096 0.135 0.046 0.120 0.146

trans-Lutein FSV-BT 0.056 0.136 0.103 0.168 0.175

trans-Zeaxanthin FSV-BT 0.019 0.027 0.031 0.048 0.048

cis-Lutein&Zeaxanthin FSV-BT 0.027 0.077 0.063 0.118 0.131

trans-Lutein&Zeaxanthin FSV-BT 0.074 0.163 0.133 0.216 0.223

Legend 

na Not available for analysis
 

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

>x Value greater than x
 

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 

L6
 

All Lab Report Page 5 / 6 
Round Robin XXIX Laboratory Results
 

% Bias Summary
 

Lab TR aT g/bT bC 

FSV-BA 2±4 0±2 4±4 6±5 

FSV-BD 4±7 -6±2 

FSV-BE -2±2 25±7 5±2 22±5 

FSV-BF 2±3 4±3 7±10 30±10 

FSV-BG -5±9 -4±6 -1±17 

FSV-BH -6±1 3±4 -4±3 6±3 

FSV-BI -4±3 0±1 -1±2 -3±3 

FSV-BJ 4±4 4±4 -1±7 9±5 

FSV-BK 0±12 -1±4 

FSV-BL 37±48 3±3 

FSV-BM -4±7 0±2 

FSV-BN 4±5 18±13 17±6 

FSV-BO -19±10 -13±13 0±13 

FSV-BP 0±6 -1±16 -20±23 

FSV-BQ -4±4 -1±4 -7±9 

FSV-BR 2±3 

FSV-BT 4±8 5±7 0±3 11±5 

FSV-BY -1±3 1±1 0±5 4±3 

FSV-BZ -21±10 -9±21 -6±4 

FSV-CA -2±9 -6±4 

FSV-CB 10±19 -4±17 -30±5 

FSV-CG -69±3 -88±0 -86±1 -78±2 

FSV-CH 26±9 25±14 -3±11 -5±11 

FSV-CJ 20±3 5±5 -20±3 

FSV-CK 6±19 6±19 -24±12 -20±15 

FSV-CM 2±2 

FSV-CO -4±4 -1±1 2±3 

FSV-CP -14±1 -11±2 

FSV-CQ 8±4 7±3 -32±22 

FSV-CR 3±4 -1±4 

FSV-CT 12±19 -5±8 9±12 

FSV-CU 4±4 -6±3 -8±10 

FSV-CV -1±1 -4±4 4±10 0±6 

FSV-CX 8±9 1±7 -19±40 

FSV-CY -1±5 0±7 8±11 

FSV-DJ -2±17 17±5 

FSV-DM 3±6 31±1 -5±6 

FSV-DS 10±17 4±5 4±4 

FSV-DX -7±5 -3±10 -40±17 

FSV-EA 6±11 -4±5 9±7 -19±3 

FSV-EB 1±5 3±9 5±6 

FSV-EC -27±5 -96±0 217±27 

FSV-EI -8±5 -11±6 -9±10 -43±9 

FSV-EJ -7±15 11±6 -9±17 -25±4 

FSV-EK 6±8 2±3 15±4 -3±5 

FSV-EN -8±5 -12±6 8±16 

FSV-EX -2±4 6±5 11±7 

FSV-FC 5±12 1±13 -3±12 5±7 

FSV-FF 1±3 26±7 

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. 

L7
 

All Lab Report Page 6 / 6 
 

 

Appendix M. Shipping Package Inserts for RR04 

The following two items were included in each package shipped to a RR04 participant: 

• Cover letter 

• Report of Analysis datasheet 

These items were attached to the shipping box. 

M1
 
 

 

 

 

 

 

 

 

 

 

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 3, 1993 

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 the original 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. If the samples arrive completely defrosted, please record the date of receipt and contact 

me immediately (301 / 975-3137). 

You should find six ampoules in the shipping container. Each ampoule contains between 0.2 and 

0.8 mg of ascorbic acid/dL of serum and each ampoule should be analyzed in duplicate by the 

method(s) used in your laboratory (preferably one measuring total ascorbic acid). 

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 15, 1993. 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 FAX your results, the number is (301) 926-8671. If you have any 

questions, I can be reached at (301) 975-3137. 

Thank you for your assistance. 

Sincerely, 

Sam A. Margolis, Ph. D. 

Research Chemist 

Organic Analytical Research Division 

Center for Analytical Chemisty 

M2
 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

REPORT OF ANALYSIS 

NAME: 

ADDRESS: 

Method of Analysis: 

Date of Analysis: 

Telephone Number: 

FAX Number: 

RESULTS (μg/mL) 

SERUM 178, VIAL# 

REPLICATE 1 

REPLICATE 2 

________ μg/mL 

________ μg/mL 

SERUM 178, VIAL# 

REPLICATE 1 

REPLICATE 2 

________ μg/mL 

________ μg/mL 

SERUM 179B, VIAL# 

REPLICATE 1 

REPLICATE 2 

________ μg/mL 

________ μg/mL 

SERUM 179B, VIAL# 

REPLICATE 1 

REPLICATE 2 

________ μg/mL 

________ μg/mL 

SERUM 180, VIAL# 

REPLICATE 1 

REPLICATE 2 

________ μg/mL 

________ μg/mL 

SERUM 180, VIAL# 

REPLICATE 1 

REPLICATE 2 

________ μg/mL 

________ μg/mL 

M3
 
 

 

 

Appendix N. Final Report for RR05 

The following ten pages are the final report for RR05 as provided to all participants. This 

report contains: 

•	 Cover letter and analysis of results. 

•	 Table 1 “Results of the Round Robin Measurement of Ascorbic Acid in Human 

Plasma”. 

•	 Table 2 “NIST Results for the Measurement of AA in Human Plasma”. 

•	 Figure 1 “Box Plot of the Round Robin Results” 

•	 Figure 2 “Distribution of the Round Robin Results for Lot 178” 

•	 Figure 3 “Distribution of the Round Robin Results for Lot 179B” 

•	 Figure 4 “Distribution of the Round Robin Results for Lot 180” 

•	 A page intended to facilitate the participants’ return of comments 

A number of the results reported in the Tables were later revised to correct for 

miscommunication of the reporting units. Since the listed results do not necessarily 

represent measurement performance, the Lab identifiers used by Dr. Margolis have been 

redacted from these Tables rather than re-coded. The reporting unit confusion impacts 

some of the conclusions discussed in the cover letter. However, the results discussed in 

the Dr. Margolis’s text have not been updated or corrected. 

The “All Lab Report” in Appendix O lists the corrected results and provides more 

extensive statistical summaries. 

N1
 
 

 

 

 

 

 

 

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 

January 27, 1994 The letter as distributed to participants has been lost. This 

version has been prepared from an extant draft. 

Dear Colleague: 

This report describes both the overall-group and your laboratory's performance in Round 

Robin IV for the measurement of ascorbic acid in human plasma. The study involve the 

duplicate analysis of four samples (two each from lots 178, 179B, and 180). Specifically, your 

package contains tabular presentations of all data submitted for ascorbic acid for Round Robin 

IV. Your results are designated "Data Set_#_" in the tables and figures. 

Table 1 provides a summary of the data submitted by fourteen laboratories (the NIST data were 

not included in the statistical analysis). One laboratory submitted two sets of measurements,
 

each done by a different method. As shown in Table 1, the percent Relative Standard Deviation 

(RSD) for all three lots ranged from 26.8 to 32.3. The intra-laboratory %RSD ranged from 3.6 to
 

9.6, indicating that the major source of variation was the interlaboratory variation. The box plot
 

in Figure 1 is a graphic summary of the results. The minimum and maximum values for each lot
 

are plotted as small solid circles, the two simple lines each span the next three “worst” 

above/below values and the center box contains the values from seven data sets. The NIST mean
 

value for ascorbic acid (AA) + dehydro-AA are represented by a circle with a T inside and the 

NIST mean for reduced AA is represented by a R inside a circle. The horizontal line in the 50%
 

boxes represents the median interlaboratory values which are slightly below the NIST values.
 

Figures 2 to 4 are plots of the distribution of the data points submitted by each laboratory for
 

each sample lot. From these plots and the data in Table 1, it is apparent that the results
 

obtained with the dinitrophenylhydrazine (DNPH) method (data sets 2 to 4), except for data set 3
 

lot 178, fall into a unique group of values which are higher than the NIST mean by
 

approximately 10 to 25 %. Similarly all but one set of data obtained by LC methods are 5 to 

15% below the NIST mean. Finally, one set of data (set 1) is exceptionally low. The high 

average mean of the DNPH measurements is not significant because of the wide distribution of
 

values but it is consistent with previous round robins and suggests that the DNPH method may
 

be positively biased. The basis of the distribution of the majority of the LC measurements below
 

the NIST mean requires further evaluation along with the large variation in the results (%RSD = 

27 to 32%). The observation that all of the gravimetrically added AA was accounted for (Table 

2) also supports the need to continue these round robins in order to reduce the measurement
 

variation.
 

The next set of samples, Round Robin V, will be shipped around the end of January or the early
 

part of February. If you are interested in participating in Round Robin V, please indicate it on 

the enclosed sheet and return it via mail or FAX to:
 

Dr. Sam Margolis, NIST - Chemistry B156 Gaithersburg, MD 20899 (301)926-8671.
 

N2 
 

If you have any questions please contact me at (301)975-3137 or FAX at (301)926-8671. 

Also on the enclosed sheet please indicate if you would like to participate in a one day workshop 

on the measurement of vitamin C to be held in conjunction with the Micronutrient Quality 

Assurance Workshop tentatively scheduled to be held at NIST in October 1994. 

Sincerely, 

Sam A. Margolis, Ph.D. 

Research Chemist 

Organic Analytical Research Division 

Chemical Science and Technology Laboratory 

Enclosures 

N3 
 

 

 

 

Method Legend 

OPD Orthophenlyenediamine 

DNPH 2,4-Dinitrophenylhydrazine 

ENZ Enzyme conversion (ascorbate oxidase) 

LC-EC Liquid chromatography with electrochemical detection 

DCIP 2,6-dichlorophenolindophenol 

N4
N5
 
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l/ 

( 

Figure 1. Box Plot of the Round Robin Results 

Figure 2. Distribution of Round Robin Results for Lot 178 

Figure 3. Distribution of Round Robin Results for Lot 179B 

Figure 4. Distribution of Round Robin Results for Lot 180 

Key for Figures 2-4: 

• First Vial; First Measurement 

+ Second Vial; First Measurement 

D First Vial: Second Measurement 

0 Second Vial;Second Measurement 

Data Set 19 are the NIST values for AA+DHAA 

Data Set 20 are the NIST values for AA 

N6
 
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N9
 
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N10
 
Dr. Margolis sent individual letters to invited study 

participants. The "Title

~", "Company

~", "Address

~", and 

"Lab No.

~" were mail-merge commands for inserting a 

participant's name, address, and laboratory code number. 

N11 
 

 

 

Appendix O. Updated “All-Lab Report” for VC-RR04 

The following two pages are an updated “All-Lab Report” for RR04. This report 

contains the same information as originally provided to all participants, with the 

following exceptions: 

•	 the participant identifiers (Lab) have been altered to ensure confidentiality of 

identification codes assigned to laboratories.. 

•	 the order in which the participant results are listed has been altered. 

•	 results have been corrected and transformed to have units of μmol/L sample. 

•	 additional summary statistics have been included. 

•	 a Legend page has been added 

O1
 
Vitamin C Round Robin 4
 

O

2

Lab Date Method 

VC-MA 16-Sep-93 HPLC-UV
 

VC-MB 24-Aug-93 AO
 

VC-MC 9-Sep-93 AO-OPD
 

VC-MD 9-Sep-93 HPLC-EC
 

VC-ME 24-Jan-94 24DNPH
 

VC-MV 13-Sep-93 HPLC-UV
 

VC-NB 7-Jan-94 HPLC-EC
 

VC-NC 13-Sep-93 HPLC-EC
 

VC-NG 14-Sep-93 HPLC-EC
 

VC-NN 3-Sep-93 24DNPH
 

VC-NP 12-Jan-94 HPLC-EC
 

VC-NS 15-Sep-93 HPLC-EC
 

VC-NT 23-Aug-93 HPLC-EC
 

VC-NW 21-Sep-93 HPLC-UV
 

NIST HPLC-EC 

178, [TAA] μmol/mL 

Mean S dup S rep S het S tot 

11.1 0.2 0.2 0.1 0.2 

11.9 0.8 1.6 0.0 1.6 

11.7 0.6 0.3 0.6 0.7 

11.7 0.6 0.1 0.6 0.6 

12.8 0.2 0.2 0.1 0.2 

9.9 0.0 0.0 0.0 

12.1 1.6 0.3 1.6 1.6 

19.6 0.6 0.2 0.6 0.6 

12.3 1.0 0.5 0.9 1.0 

15.8 1.0 3.5 0.0 3.5 

11.2 1.4 0.1 1.4 1.4 

12.1 0.6 0.6 0.6 

4.8 0.0 0.0 0.0 0.0 

9.2 0.0 0.4 0.0 0.4 

13.5 0.2 0.2 0.2 0.3 

180, [TA

Mean S dup 

18.4 0.3 

18.0 1.8 

23.0 2.0 

20.9 1.6 

20.7 0.0 

14.5 0.5 

22.0 0.8 

28.0 0.1 

22.2 1.8 

37.3 0.6 

20.1 0.0 

19.9 1.2 

6.8 0.0 

16.3 0.7 

21.3 0.1 

179B, [TAA] μmol/mL 

Mean S dup S rep S het S tot 

64.4 0.0 1.0 0.0 1.0 

64.7 0.1 0.9 0.0 0.9 

101.5 1.1 4.7 0.0 4.7 

68.1 1.5 1.8 0.8 2.0 

66.5 1.3 2.0 0.0 2.0 

48.6 1.5 0.7 0.7 

87.5 1.3 1.3 0.9 1.6 

89.6 0.4 0.5 0.1 0.5 

77.9 6.5 1.8 6.4 6.6 

90.3 3.6 1.4 3.5 3.8 

63.4 0.3 0.8 0.0 0.8 

74.7 2.4 1.4 1.4 

19.3 0.2 0.3 0.0 0.3 

60.1 1.1 0.3 1.1 1.1 

77.2 0.5 0.0 0.5 0.5 

N 14 14 14 

Min 4.8 0.0 0.0 0.0 0.0 19.3 0.0 0.3 0.0 0.3 6.8 0.0 

Median 11.8 0.6 0.3 0.4 0.6 67.3 1.2 1.2 0.1 1.3 20.4 0.7 

Max 19.6 1.6 3.5 1.6 3.5 101.5 6.5 4.7 6.4 6.6 37.3 2.0 

eSD 1.0 13.3 3.3 

eCV 9 20 16 

Revised "All Lab Report" 
Datasets 

Each participant typically reported two replicate measurements for each of two duplicate 

vials for each test sample. However, occasionally only one vial of each pair was 

evaluated or a single result was reported for each of the duplicate vials. 

Legend 

Lab	 Laboratory Code 

Date	 Date that the results were received at NIST 

Method Type of assay 

AO Ascorbate oxidase 

24DNPH 2,4-Dinitrophenylhydrazine 

EC Electrochemical detector 

HPLC Liquid chromatography 

OPD Orthophenlyenediamine 

UV Ultraviolet absorbance 

Mean Mean of duplicate means 

Sdup Standard deviation of duplicate means 

Srep Pooled standard deviation of replicates 

2 2 Shet	 Estimated sample heterogeneity, ටMAX൫0, Sdup − Shet൯

2 2 Stot	 Estimated standard deviation of the mean, ට൫Sdup + Srep൯⁄n, 

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

N The number of participants 

Min Minimum value in the column 

Median Median value in the column 

Max Maximum value in the column 

eSD Adjusted median absolute deviation from the median (MADe) 

eCV Estimated coefficient of variation, 100*eSD/Median 

O3