NISTIR 7880-27 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1997 

Comparability Studies 

Results for Round Robin XXXIX, XL, and XLI 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 10 Ascorbic Acid in Human Serum 

David L. Duewer 

Margaret C. Kline 

Sam A. Margolis (Retired) 

Katherine E. Sharpless 

Jeanice B. Thomas 

 

 

 

 

 

NISTIR 7880-27 

NIST Micronutrients Measurement 

Quality Assurance Program 

Winter, Spring, and Fall 1997 

Comparability Studies 

Results for Round Robin XXXIX, XL, and XLI 

Fat-Soluble Vitamins and Carotenoids in Human Serum 

and Round Robin 10 Ascorbic Acid in Human Serum 

David L. Duewer 

Sam A. Margolis (Retired) 

Katherine E. Sharpless 

Jeanice B. Thomas 

Chemical Sciences Division 

Materials Measurement Laboratory 

Margaret C. Kline 

Biomolecular Measurement Division 

Material Measurement Laboratory 

July, 2013 

U.S. Department of Commerce 

Penny Pritzker, Secretary 

National Institute of Standards and Technology 

Patrick D. Gallagher, Under Secretary of Commerce for Standards and Technology and 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 1997 MMQAP measurement comparability improvement studies: 1) Round 

Robin XXXIX Fat-Soluble Vitamins and Carotenoids in Human Serum, 2) Round Robin XL FatSoluble Vitamins and Carotenoids in Human Serum, 3) Round Robin XLI Fat-Soluble Vitamins and 

Carotenoids in Human Serum, and 4) Round Robin 10 Ascorbic Acid in Human Serum. The 

materials for Round Robin XXXIX were shipped to participants in January 1997; participants were 

requested to provide their measurement results by March 21, 1997. The materials for Round Robin 

XL were shipped to participants in April 1997; participants were requested to provide their 

measurement results by June 13, 1997. The materials for Round Robin XLI were shipped to 

participants in July 1997; participants were requested to provide their measurement results by 

September 19, 1997. The sample materials for Round Robin 10 were distributed in November 1996 

with results due by January 15, 1997. 

Keywords 

Human Serum 

Retinol, α-Tocopherol, γ-Tocopherol, Total and Trans-β-Carotene, SRM 968b 

Ascorbic Acid 

iii 
 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

Table of Contents 

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

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

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

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

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

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

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

Round Robin 10: Vitamin C in Human Serum............................................................................... 3
 

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

Appendix A. Shipping Package Inserts for RR39........................................................................ A1
 

Appendix B. Final Report for RR39 ..............................................................................................B1
 

Appendix C. “All-Lab Report” for RR39 ......................................................................................C1
 

Appendix D. “Individualized Report” for RR39 ......................................................................... D1
 

Appendix E. Shipping Package Inserts for RR40 ......................................................................... E1
 

Appendix F. Final Report for RR40............................................................................................... F1
 

Appendix G. “All-Lab Report” for RR40...................................................................................... G1
 

Appendix H. “Individualized Report” for RR40 .......................................................................... H1
 

Appendix I. Shipping Package Inserts for RR41 ........................................................................... I1
 

Appendix J. Final Report for RR41 ................................................................................................ J1
 

Appendix K. “All-Lab Report” for RR41..................................................................................... K1
 

Appendix L. “Individualized Report” for RR41........................................................................... L1
 

Appendix M. Shipping Package Inserts for RR10 ....................................................................... M1
 

Appendix N. Final Report for RR10 ............................................................................................. N1
 

Appendix O. “All Lab Report” for RR10 ..................................................................................... 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 total 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 XXXIX: Fat-Soluble Vitamins and Carotenoids in Human Serum 

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

XXXIX comparability study (hereafter referred to as RR39) received four lyophilized human serum 

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

vial of each serum. These sera were shipped on dry ice to participants in January 1997. The 

communication materials included in the sample shipment are provided 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 many 

participants report values for non-target analytes. 

The final report delivered to every participant in RR39 consists of three documents: 

•	 A cover letter and summary report for the current study that describes the samples, our 

analysis of the participants’ results, and a detailed analysis of measurements made by NIST 

analysts. This cover letter and summary report is reproduced as Appendix B. 

•	 The “All-Lab Report” that lists all of the reported measurement results, a number of 

consensus statistics for analytes reported by more than one participant, and the mean median 

and pooled SD from any prior distributions of the serum. This report also provides a 

numerical “score card” for each participant’s measurement comparability for the more 

commonly reported analytes. This report is reproduced as Appendix C. 

1
 
 

 

 

 

 

 

 

 

 

 

 

•	 An “Individualized Report” that graphically analyzes each participant’s results for selected 

analytes. This report also provides a graphical summary of their measurement comparability. 

The graphical tools used in this report are described in detail elsewhere [3]. An example 

“Individualized Report” is reproduced as Appendix D. 

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

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

XL comparability study (hereafter referred to as RR40) received four lyophilized human serum test 

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

of each material. These sample materials were shipped on dry ice to participants in April 1997. The 

communication materials included in the sample shipment are provided 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 many 

participants report values for non-target analytes. 

The final report delivered to every participant in RR40 consists of three documents: 

•	 A cover letter and summary report for the current study that describes the samples, our 

analysis of the participants’ results, and a detailed analysis of measurements made by NIST 

analysts. This cover letter and summary report is reproduced as Appendix F. 

•	 The “All-Lab Report” that lists all of the reported measurement results, a number of 

consensus statistics for analytes reported by more than one participant, and the mean median 

and pooled SD from any prior distributions of the serum. This report also provides a 

numerical “score card” for each participant’s measurement comparability for the more 

commonly reported analytes. This report is reproduced as Appendix G. 

•	 An “Individualized Report” that graphically analyzes each participant’s results for selected 

analytes. This report also provides a graphical summary of their measurement comparability. 

The graphical tools used in this report are described in detail elsewhere [3]. An example 

“Individualized Report” is reproduced as Appendix H. 

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

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

XLI comparability study (hereafter referred to as RR41) received four lyophilized human serum test 

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

of each material. These sample materials were shipped on dry ice to participants in July 1997. The 

communication materials included in the sample shipment are provided 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 many 

participants report values for non-target analytes. 

The final report delivered to every participant in RR41 consists of three documents: 

2
 
 

 

 

 

 

 

 

•	 A cover letter for the current study, a brief description of the other document, and a 

discussion of our analysis of overall results that may be of broad interest. This cover letter is 

reproduced as Appendix J. 

•	 The “All-Lab Report” that lists all of the reported measurement results, a number of 

consensus statistics for analytes reported by more than one participant, and the mean median 

and pooled SD from any prior distributions of the serum. This report also provides a 

numerical “score card” for each participant’s measurement comparability for the more 

commonly reported analytes. This report is reproduced as Appendix K. 

•	 An “Individualized Report” that graphically analyzes each participant’s results for selected 

analytes. This report also provides a graphical summary of their measurement comparability. 

The graphical tools used in this report are described in detail elsewhere [3]. An example 

“Individualized Report” is reproduced as Appendix L. 

Round Robin 10: Vitamin C in Human Serum 

Participants in the MMQAP Vitamin C in Human Serum Round Robin 10 comparability study 

(hereafter referred to as RR10) received four frozen serum test samples and a solid ascorbic acid 

control material for analysis. These sample materials were shipped on dry ice to participants in 

September 1997. The communication materials included in the sample shipment are provided 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. Participants were also asked to prepare and evaluate a standard solution of 50 

μmol ascorbic acid (AA) per L solution of 5 % by mass metaphosphoric acid. 

The final report delivered to all participants in RR10 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 RR10, Appendix O is a modified “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 RR10. 

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
 
3 Duewer DL, Kline MC, Sharpless KE, Brown Thomas J, Gary KT, Sowell AL. Micronutrients 

Measurement Quality Assurance Program: Helping Participants Use Interlaboratory Comparison 

Exercise Results to Improve Their Long-Term Measurement Performance. Anal Chem 

1999;71(9):1870-1878. 

4
 
 

Appendix A. Shipping Package Inserts for RR39 

The following two items were included in each package shipped to an RR39 participant: 

• Cover letter 

• Datasheet 

The cover letter and datasheet were enclosed in a sealed waterproof bag along with the 

samples themselves. 

A1
March 4, 1997: 

UNITED STATES DEPARTMENT OF COMMERCE 

Nationd Institute of Standards and Technology 

Gaithersburg, Maryland 20899-

Enclosed is the set of samples for the first quality assurance round robin exercise (Round Robin XXXIX) 

for FY97. You will find one vial of each of four lyophilized serum samples 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. If an obtained value is below your limit of quantitation, please indicate this result on 

the form by using NQ (Not Quantitated). For analytes not measured, please leave a blank. Results are 

due to NIST by March 21, 1997. Results received two weeks after the due date will not be included in the 

summary report for this round robin study. Written feedback concerning the study will be provided 

around April 18, 1997. If you joined the program after the scheduled distribution date, please submit your 

results as promptly as possible. You will be provided feedback within two weeks from receipt of your 

results. 

Samples should be reconstituted with 1.0 mL ofHPLC-grade water or equivalent. We recommend that 

dissolution be facilitated with 3 to 5 min 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 that 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 retinal in most LC systems creating analytical problems.) Pipette a known 

volume of serum from the vial for analysis. (The final volume of the reconstituted sample is greater than 

1.0 mL.) For consistency, we request that laboratories use the following absorptivities (E 1 % cm) in 

ethanol: retinal, 1850 at 325 nm; retinyl palmitate, 975 at 325 nm; a-tocopherol, 75.8 at 292 nm; 

y-tocopherol, 91.4 at 298 nm; a.-carotene, 2800 at 444 nm (in hexane); ~-carotene, 2560 at 450 nm (in 

ethanol), 2592 at 452 nm (in hexane); lycopene, 3450 at 472 run (in hexane). 

Please mail or fax your results for Round Robin XXXIX to: 

Micronutrients Measurement Quality Assurance Program 

NIST 

Bldg. 222, Rm. B208 

Gaithersburg, MD 20899 

Fax: (301) 977-0685 

If you have questions regarding this round robin exercise, please call me at (301) 975-3120; 

e-mail me atjeanice.bro thomas@nist.gov; or mail/fax queries to the above address. 

nalytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

cc: S. Wise 

(Most participants received samples in January, 1997)
	

A2
 

 

 

 

NIST/NCI
 

Micronutrients Measurement Quality Assurance Program
 

Round Robin XXXIX Results from Laboratory #_____ 

Serum 

Analyte 227 228 229 230 Units* 

retinol 

retinyl palmitate 

α-tocopherol 

γ-tocopherol 

δ-tocopherol 

total β-carotene 

trans-β-carotene 

total cis-β-carotene 

total α-carotene 

trans-α-carotene 

total lycopene 

trans-lycopene 

β-cryptoxanthin 

lutein 

zeaxanthin 

lutein&zeaxanthin 

Other Analytes?
 

* We prefer mg/mL 

Today's Date: 

Comments? 

Mail: MMQAP, 222/B208 

NIST Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899 March 15, 1997 Email: David.Duewer@NIST.gov 

A3
Appendix B. Final Report for RR39

The following 15 pages are the final report as provided to all participants: 

•	 Cover letter 

•	 A “Report of Analysis” that: 

o	 describes the nature of the test samples and details any previous distributions 

o	 summarizes aspects of the study that we believe may be of interest to the 

participants 

o	 details the analysis of the NIST results 

B1
 
Aprill?, 1997 

Dear Colleague: 

Enclosed is the summary report of the results for Round Robin XXXIX (RR39). Included in this 

report are: a summary of data for all laboratories; the measurement comparability summary for 

evaluating laboratory performance; a summary of individual laboratory performance for the past 

three years; a summary of the interlaboratory accuracy and precision over the same period of 

time for the measurement ofretinol, ex- and y-tocopherol, and trans- and total ~-carotene; and a 

graphical summary of the NIST assigned value vs. your laboratory value for these analytes. As 

in previous reports, the NIST assigned values are derived from the equally weighted results from 

the analyses performed by NIST and the laboratories that participated in this interlaboratory 

comparison exercise. 

While the information in this report is much the same as in previous reports, the old "Report of 

(Meta)Analysis" and "Lies, Damned Lies, and Statistics" have been replaced with an "Analysis 

of Results" that more concisely describes the nature of the samples; the qualitative observations 

made by the participants and NIST analysts; actions taken in response to these observations; 

quantitative analysis for value and uncertainty assignments; and a summary of the overall 

laboratory performance drawn from the quantitative results. 

The experimental design for this interlaboratory comparison exercise is summarized below. The 

four serum samples (Sera 227-230) distributed in RR39 address the following issues: 

• Serum and Measurement Stability. Serum 227 is the high level component of SRM® 968b 

and was previously distributed as Sera 202 in RR32 and 210 in RR34. Reanalysis of such wellcharacterized materials documents both the continued stability of the material and of the 

"absolute accuracy" of the analyte level assignments. No significant changes in analyte stability 

were observed. 

• Measurement Precision and Concordance. Serum 228 was previously distributed as the 

blind duplicate Sera 223 and 225 in RR38. Reanalysis of this material contributes to our ongoing study of the sources of"long-term" within-laboratory measurement precision and 

among-laboratory measurement concordance. We will continue to explore within-laboratory 

measurement performance for discussion at our next quality assurance (QA) workshop. 

• Analyte Augmentation Techniques. Sera 229 and 230 were prepared from the same "low 

normal" serum pool. We attempted to augment many of the commonly reported analytes to a 

"high" level in one of the two sera, with mixed success, ranging from nearly 100% of the 

intended levels for retinal, 5-, y-, and ex-tocopherol, lutein, and zeaxanthin to about 0% for 

P-carotene. We will continue to evaluate our augmentation techniques to determine why there 

was a complete loss of P-carotene and poor incorporation of ex-carotene. 

B2
 
In this interlaboratory comparison exercise, the retinyl palmitate level was augmented in all four 

samples. While fairly high levels (about 0.05, 0.1, and 0.15 μg/mL) were achieved in the other 

three sera, measurement performance was acceptable only for the highest level (0.2 μg/mL) in 

Serum 227. 

Serum 229 was augmented to a very high zeaxanthin level and Serum 230 was augmented to a 

very high lutein level. While most laboratories that separately report lutein and zeaxanthin did 

quite well, several laboratories misreported the high zeaxanthin in Serum 229 as lutein. If your 

laboratory had difficulty with this analyte pair, we recommend that you report a combined value 

for "lutein and zeaxanthin" rather than for the individual analytes. 

Data for evaluating laboratory performance in RR39 are provided in the comparability summary 

(Score Card) on page 6 of the "All Lab Report." The criteria used to evaluate laboratory 

performance are as follows: results rated 1 (within 1 SD of the assigned value) indicate 

EXCEPTIONAL performance, results rated 2 (within 2 SD) indicate ACCEPT ABLE 

performance, results rated 3 (within 3 SD of the assigned value) are MARGINAL, and those 

rated 4 (> 3 SD from the assigned value) indicate POOR performance relative to the current stateof-the-practice for these measurements. 

If you have concerns regarding your laboratory performance or were rated "POOR" based on the 

criteria stated above, we suggest that you obtain a unit of SRM 968b, Fat-Soluble Vitamins and 

Cholesterol in Human Serum, and analyze all three levels. If, with minor modifications, your 

measured values do not agree with the certified values, we suggest that you contact us for 

consultation. 

Samples for RR40 and the food Round Robin 6 (coordinated by Dr. Katherine Sharpless at 

3011975-3121) will be shipped during the last week of April. Results for both exercises are due 

June 13; feedback to labs will be provided around July 25. 

The Micronutrients Measurement QA Workshop will be held prior to the American Association 

for Clinical Chemistry meeting on July 20, 1997 at the Best Western American Hotel in Atlanta, 

Georgia. You will be provided with further details about the workshop in about two weeks. 

The QA homepage is now available! The web-site address for the homepage is: 

http://www.cstl.nist.gov/nist839/839.02/qahome.htm. Your comments and suggestions are 

welcomed. 

Enclosed is a copy of our first publication on longitudinal QA analysis: NIST/NCI 

Micronutrients Measurement Quality Assurance Program: Measurement Repeatabilities 

and Reproducibilities for Fat-Soluble Vitamin-Related Compounds in Human Sera, 

Duewer, D.L., et al., Anal Chem, 69 (1997) 1406-1413. 

B3
 
The following are forthcoming publications: 

• Liquid Chromatographic Measurement of L-Ascorbic Acid and D-Ascorbic Acid in 

Biological Samples, Margolis, S.A. and Schapira, R.M., J. Chromatogr. B, 690 (1997) 25-33. 

•Certification of Nutrients in Standard Reference Material 1846: Infant Formula, 

Sharpless, K. E., et al., J. AOAC, in press. 

• "Vitamin A," In: Laborato:ry Medicine: A Scientific and Mana~erial Infobase, Sharpless, K.E., 

Brown Thomas, J., Turley, C.P., and Brewster, M.A., version 2.6, A. J. Pesce and L.A. 

Kaplan, editors, Pesce Kaplan Publishers, Cincinnati, OH, June 1997. 

• "Vitamin E," In: Laborato:ry Medicine: A Scientific and Mana~erial Infobase, Sharpless, K.E., 

Brown Thomas, J., Turley, C.P., and Brewster, M.A., version 2.6, A. J. Pesce and L.A. 

Kaplan, editors, Pesce Kaplan Publishers, Cincinnati, OH, June 1997. 

Reprints of the above publications will be sent to you pending availability. If you have any 

questions, please contact me at 3011975-3120; FAX: 3011977-0685; e-mail: 

j eanice.brownthomas@nist.gov. 

E!=l~ Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

cc: W. May 

S. Wise 

B4
 
' " 

Analysis of Results Round Robin XXXIX: Sera 227-230 Paac l 

Analysis of N2M2QAP Round Robin XXXIX Results: Sera 227 to 230 

Background: The following four samples were distributed in RR39 

Serum 227: the "high level" component of Fat-Soluble Vitamins in Serum SRM~ 968b. It 

was previously distributed as serum 202 in RR32 (9/94) and serum 210 in RR34 (6/95). This 

material was prepared from high-carotenoid serum pools and was augmented with retinol, 

retinyl palmitate (RP), and the tocopherols. 

Serum 228: this was distributed as the blind duplicate sera 223 and 225 in RR38 (9/96). This 

material was prepared from a natural "normal" serum pool, lightly augmented with RP. 

Serum 229: a new serum, prepared from a natural "low" serum pool. It was augmented with 

RP, y- and 8-tocopherol, trans-lycopene, and lutein. (We intended to augment this serum with 

trans-p-carotene ... and the notebook says we augmented it ... but if we actually augmented it, 

it sure didn't go into solution!) 

Serum 230: a new serum, prepared from the same natural "low" serum pool used for serum 

229. It was augmented with retinol, RP, a- and 6-tocopherol, trans-a-carotene, translycopene, p-cryptoxanthin, and zeaxanthin. 

Qualitative Results: The following observations were noted in the RR39 reports: 

Two participants reported a small unknown peak eluting in the retinoVS-tocopherol region for 

both sera 229 and 230, with one participant suspecting the presence of cis-retinyl acetate. 

There is some evidence that these participants' results were degraded by this interferant. 

Analyst NIST3 confirms the presence of a small peak prior to the retinol peak that is 

compatible with the possible presence of a retinyl acetate isomer. 

Action: We used a different source of RP for augmenting the RR40 samples. If this does 

not banish the interferant, we will need to more completely characterize all of the 

augmentation materials. 

One participant noted the presence of a small amount of the freeze-dried material clinging to 

the vial stoppers of two samples. · All results from this laboratory were within 2 SD of the 

median, with no correspondence between the magnitude of the measurement deviations and 

the suspect samples. 

Action: None required. There is no evidence of contamination from the vial stoppers. 

(Analyst NIST3 notes that this is a fairly common occurance, and that you "just 

try to swoosh it down with the H20.") 

One participant noted our use of clear vials while all the analytes are known to be 

photosensitive. 

Action: We used 2.0 mL amber borosilicate vials for the RR40 samples instead of the old 

3.5 mL flint glass vials. While the smaller volume of the new vials is of concern, 

only 2.0 mL and 5.0 mL amber vials are readily available. The smaller diameter 

and more regular shape of the 2.0 mL ambers does permit many more samples to 

be prepared in a single freeze-dryer batch. If the RR40 samples prove acceptable, 

we intend to use these amber vials for all future serum samples. 

One participant noted with enthusiasm our success at achieving high lutein and zeaxanthin 

levels, and pointed to the need for higher a-carotene and p-cryptoxanthin levels. 

Action: We're trying, we're trying ... 

B5
 
Analysis of Results Round Robin XXXIX: Sera 227-230 Page 2 

Quantitative Results: Table l, NIST Data and Value/Uncertainty Assignments, presents all 

NIST data, summary statistics for the NIST data, summary results for RR39, and the NIST 

assigned values and uncertainties. The assigned values and uncertainties for each analyte in 

each serum are summarized in Table 2, Summary of NIST Assigned Values/Uncertainties. 

The entries in Tables 1 and 2 are defined as follows: 

Individual NIST Analyst Data and Summazy Statistics 

A: 1 to C:2 two aliquots (" l" and "2") of three vials (A, B, and C) of each serum were 

extracted and analyzed. Each analyst analyzed a separate set of three vials. 

Ilx number of quantitative values for this analyte for this serum for this analyst 

Me8Ilx arithmetic average 

SD11 simple standard deviation 

SDrepx within-vial pooled standard deviation, reflecting variation in extraction, 

chromatography, peak integration, etc. 

SD11ea among-sample standard deviation, reflecting heterogeneity in preparing and 

reconstituting the serum samples 

SDNJSTx ~SD~px + SD~cx, total standard deviation. This value is~ SD11 , as sample 

replicates reduce the true degrees of freedom. 

CV NISTx 100 x SD NJST/Mean11 

NIST Summazy Statistics 

o number of quantitative values for this analyte for this serum 

Mean (MeanNJST1 + MeanNJSn)/2 or MeanNJsn for analytes that NISTl did not report 

SDrep within-vial pooled standard deviation 

SD11et among-sample standard deviation 

SDan1 between-analyst standard deviation. This is the residual standard deviation for 

regression of NIST3's Mean11 values to NISTl 's or, for analytes that NISTl did 

not report, to the interlaboratory Median (see below). The model used to 

determine SD1111 is defined to the right of this block. Details include: model used, 

parameters and standard errors on the parameters, and R 2 • 

SDNJST ~SD~ +SD~ + SD~1 , total standard deviation for NIST analyses. 

CV NIST 100 x SD NJs,JMean 

Round Robin XXXIX Summazy Statistics 

00 number of non-NIST laboratories reporting quantitative values. for this analyte 

for this serum in this Round Robin 

Median0 median of the reported values 

eSD0 0.741 x InterQuartile Range (IQR) 

B6
 
Analysis of Results Round Robin XXXIX: Sera 227-230 PapJ 

P(n=p) TDIST( IMediann - MedianPl~nn + nP - 2 . ) ....,...-------..-..:==-==-=====--t ~+nD ·2, 2-tail 

(<nn - l)eSD! + (nP -l)eSD!f_l + _!_) 

\ nn nP 

This is the approximate probability that the current median is the same as it was 

in its initial distribution. Where the hypothesis that Mediann = Medi~ can be 

rejected with 95% confidence, the P(n=p) value is flagged with an"*". TDIST 

is Excel~'s student's t function. 

( eSD2 ) P(n<p) FOIST --; , n0 -l, ~-1 

eSD0 

This represents the approximate probability that the current interlaboratory 

variance is smaller than it was in its initial distribution. Where the hypothesis 

that eSD0 < eSD& can be rejected with 95% confidence, the P(n<p) value is 

flagged with an *". FOIST is Excel®' s F-distribution function. 

SD1..,. ~eSD! -SD~ S'f, the residual non-NIST interlaboratory biases after correction 

for measurement-, sampl~. and NIST-analyst-related sources of variance. When 

SDNIST is greater than eSDD, SDlab, = 0. 

CV 1ab1 100 x SD...JMedi81\ 

NIST Assiened Values and Uncertainties 

NA V (Mean + Median0 ) I 2, our best guess of the "true" analyte level 

NAU Maximum( 0.05 x NA V, ~SD~15T +SD~ ), our best guess for the "true" 

interlaboratory standard deviation characterizing measurement, sample 

heterogeneity, interanalyst, and interlaboratory sources of variation. When SDlabl 

could not be determined, NAU is estimated as 

Maximum(O.lOxNAV, ~2 SD~). 

CV lOOxNAU /NAV 

xCV 100 x ~L~ + ( B0 x NA V81 )2 I NA V, the CV we expect for a given NAV. Lqc, B0, 

and 81 are analyte-specific constants, determined from empirical analysis of the 

historical relationship between NAV and NAU for the specific analyte. 

Measurement Performance Summary: The following is based on results presented in Table 

1 of this report and the "Individualized Report" page 7 and 8 summary graphs: 

Serum 227. hi&h-level SRM 968b. stability: There is no significant difference in the level or 

measurement variability of any analyte among the three analyses of this material (sera 202, 

210, and 227). 

Action: Thankfully, none required. 

Serum 228 stability: There is some evidence of increased measurement variability for total 

~-carotene, a-carotene, and zeaxanthin in the blind-duplicate material from RR38 (sera 223, 

225, and 228). Measurement variability for these analytes is significantly higher when 

B7
 
Analysis of Results Round Robin XX.XIX: Sera 227-230 

compared to results from either serum 223 or serum 225 alone; however, the increase largely 

disappears when the results for the sera 223 and 225 blind duplicates are combined. 

Action: It is quite plausible that augmented serum is less stable than the "native" sera we 

have previously studied. We must give serious thought as to the best use of our 

limited remaining stock of this material, but some extended analysis will be done! 

We will include the data from this trio of samples in any future extended data 

analysis of blind replicate samples. 

Sera 229 and 230 homo&eneity: None of the SDbec values are a much larger than expected 

component of SDNIST. Thus, these sera are "homogenous" (rather, no analyte in either serum 

229 or 230 is unusually heterogeneous). Further, the observed CV is no larger than expected 

(xCV) for retinol, RP, y-tocopherol, total p-carotene, P-cryptoxanthin, and total lycopene. 

However, one or both sera have larger than expected CVs for cx-tocopherol, tran.t-p-carotene, 

and total ex-carotene. This may reflect interference from the (putative) retinyl acetate isomer 

(see the "qualitative" section) noted in these sera, some interaction among the tocopherols, or 

incorrect xCV parameters (see: Anal Chem 1997:69, 1406-1413). 

Action: We will revisit the xCV parameters before July, 1997, paying particular attention 

to potential interactions among the tocopherols. We should have sufficient 

experience to obtain xCV parameters for a few more analytes, as well. 

Retinyl palmitate: The CV for serum 227, NA V = 0.23 μg/mL, was a much better than 

expected 11 %. The CV s for the next-highest level, serum 230 (NA V = 0.17 μg/mL) is 

expectedly high at 31 %. 

Action: RP remains analytically challenging. We need >0.25 μg/mL levels in several 

different samples before we can reliably identify the limit of quantitative 

comparison, Lqc, for this analyte. We'll try to find/make them! 

"Lutein." "zeaxanthin." and "lutein&zeaxanthin": The CV labs for lutein in serum 229 is very 

large (200% !). This results from several laboratories mis-identifying the large zeaxanthin 

component of this material. The zeaxanthin CVs are fairly small in both materials (-17%), 

and the variability of the combined "lutein&zeaxanthin" results appear quite acceptably small. 

The values for this combination "analyte" are, however, a composite of actual combinedmeasurements and simple additions of results for the individual analyte. 

Action: While individual laboratories perform well, interlaboratory comparisons of lutein 

or zeaxanthin are not yet reliable. The combination of lutein and zeaxanthin levels 

is more analytically meaningful. 

Dave Duewer 

Research Chemist 

David.Duewer@NIST.gov 

-~~L· 

Margaret Kline 

Research Biologist 

Margaret.Kline@NIST.gov 

B8
 
Analysis Results Round Robin XXXIX: Sera 227-230 s 

Table I 

NIST Data and Value/Uncertainty Assignments 

Retinol Retinyl Palmitate 

NISTl NIST3 NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean, 

so. 

so...,. 

sobcU 

227 

0.857 

0.907 

0.910 

0.866 

0.902 

0.894 

6 

0.889 

0.023 

0.028 

0.008 

228 

0.515 

0.497 

0.506 

0.512 

0.479 

0.459 

6 

0.494 

0.022 

O.ot 1 

0.022 

229 230 

0.396 0.644 

0.394 0.665 

0.381 0.695 

0.393 0.625 

0.383 0.668 

0.384 0.647 

6 6 

0.388 0.657 

0.006 0.024 

0.005 0.031 

0.006 0.003 

227 228 229 230 227 228 229 230 

0.913 0.484 0.359 0.632 0.246 

0.862 0.481 0.358 0.632 0.261 

0.836 0.465 0.353 0.628 0.258 

0.877 0.465 0.353 0.610 0.225 

0.848 0.488 0.357 0.622 0.245 

0.886 0.474 0.345 0.644 0.251 

6 6 6 6 6 0 0 0 

0.870 0.476 0.354 0.628 0.248 

0.028 0.010 0.005 O.otl 0.013 

0.031 0.006 0.005 O.ot 1 O.ot5 

0.016 0.010 0.004 0.008 0.006 

soNIST. 0.029 0.025 0.008 0.031 o.035 0.011 o.006 0.014 0.016 

cvNIST. 3.2 5.o t.9 4.7 4.o 2.4 1.1 2.2 6.4 

·n 

Mean 

SD..., 

SI>i..c 

SD1111 

NIST 

12 12 12 

0.880 0.485 0.371 

0.030 0.008 0.003 

0.011 0.016 0.006 

0.010 0.010 0.010 

12 

0.643 

0.023 

0.007 

0.010 

s~ 0.033 0.021 0.012 0.026 

CVNIST 3.8 4.3 3.2 4.0 

RR XXXll XXXVID 

NIST3=a+b*NIST1 

a: -0.036 ±0.017 

b: 1.022 ±0.027 

R2: 0.999 

Serum 202 223 i-.;;.--........-......_. <--Previous Results--> 

Op 40 46 

Median, 0.879 0.496 

eSDP 0.080 0.038 

RRXXXIX 

n,, 

Median. 

eso. 

P(n=p) 

P(n<p) 

227 228 

47 48 

0.859 0.491 

0.056 0.032 

0.95 0.98 

0.99 0.86 

229 230 

48 48 

0.383 0.687 

0.036 0.045 

SD11111 0.045 0.025 0.033 0.037 

CV11111 5.2 5.1 8.7 5.4 

NA V 0.869 0.488 

NAU 0.056 0.032 

CV 6.4 6.7 

xCV 8.9 8.8 

(39 _dll INIS1'lll 

0.377 0.665 

0.036 0.045 

9.4 6.8 

9.1 8.7 

<-Current Results -> 

<-Assignments-> 

NIST 

12 5 6 6 

0.215 0.045 0.078 0.152 

0.019 0.008 0.007 0.004 

0.015 0.012 0.010 0.007 

0.003 0.003 0.003 0.003 

0.024 0.014 0.013 0.008 

11 32 16 5.4 

XXXll xxxvw 

202 223 

9 15 

0.263 0.084 

0.028 0.047 

RRXXXIX 

227 228 229 230 

12 12 12 12 

0.241 0.086 0.119 0.192 

0.019 0.039 0.028 0.054 

0.68 0.99 

0.90 0.75 

0 0.036 0.025 0.053 

0 42 21 28 

0.228 0.065 

0.024 0.039 

11 59 

23 42 

0.098 

0.028 

28 

32 

0.172 

0.054 

31 

24 

227 228 229 230 

0.160 0.035 0.078 0.149 

0.178 0.034 0.092 0.157 

0.217 0.063 0.078 0.147 

0.180 0.050 0.085 0.144 

0.150 0.041 0.060 0.172 

0.204 0.072 0.145 

6 5 6 6 

0.181 0.045 0.078 0.152 

0.025 0.012 0.011 O.Oll 

0.028 0.005 0.008 O.Oll 

0.015 0.012 0.010 0.007 

0.032 0.013 0.013 0.013 

17 28 17 8.6 

NIST3=a+b*Median 

a: -0.028 ±0.004 

b: 0.869 ±0.027 

R2: 0.998 

B9
 
Analysis Results 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean1 

so. 

so_ 

so ...... 

227 

17.4 

17.4 

17.S 

17.6 

17.8 

17.S 

6 

17.S 

0.1 

0.1 

0.1 

Round Robin XXXIX: Sera 227-230 

Table 1 

NIST Data and Value/Uncertainty Assignments 

a· Tocopherol y-Tocopherol 

NISTI NIST3 NISTI 

228 229 230 227 228 229 230 227 228 229 230 227 

8.17 7.31 9.9 16.6 7.08 6.70 9.6 3.57 1.69 4.29 1.30 3.30 

7.87 1.lS 10.4 16.7 7.36 6.41 10.S 3.S4 1.73 4.30 1.28 3.38 

8.S7 1.lS 11.0 17.4 7.29 6.20 10.1 3.61 l.S1 4.26 1.34 3.41 

8.12 7.11 10.S 17.7 7.20 6.62 9.6 3.34 1.73 4.37 1.28 3.43 

8.44 1.SS 10.6 18.0 7.04 S.83 10.2 3.76 l.6S 4.68 l.3S 3.SO 

7.96 7.02 10.6 17.3 7.19 6.37 10.5 3.75 1.74 4.12 1.34 3.S3 

6 6 6 6 6 6 6 6 6 6 6 6 

8.19 7.21 10.S 17.3 7.19 6.3S 10.1 3.S9 1.68 4.34 1.32 3.43 

0.27 0.19 0.3 o.s 0.12 0.32 0.4 0.15 0.07 0.19 0.03 0.08 

0.30 0.23 0.3 0.3 0.14 0.31 0.4 0.11 0.08 0.23 0.03 0.04 

0.16 0.08 0.3 0.6 0.07 0.23 0.2 0.14 0.03 0.05 0.03 0.08 

6 

NIST3 

228 229 230 

1.53 4.11 1.02 

I.SS 3.93 1.12 

l.S9 3.98 1.13 

1.52 3.91 1.11 

l.S3 3.79 1.18 

l.S9 3.81 1.04 

6 6 6 

I.SS 3.92 1.10 

0.03 0.12 0.06 

0.04 0.08 0.07 

0.01 0.11 0.03 

SI>msr1 0.2 0.34 0.24 0.4 0.6 0.15 0.38 0.5 0.18 0.08 0.24 0.04 0.09 0.04 0.14 0.08 

CVNim 1.0 4.1 3.4 3.9 3.6 2.1 6.1 4.6 5.0 4.9 5.5 3.0 2.7 2.6 3.S 6.9 

n 

Mean 

SD..., 

SD.,. 

SD..i 

S~IST 

CVNIST 

RR 

NIST 

12 12 12 

17.4 7.69 6.78 

0.1 0.23 0.25 

o.s 0.36 0.33 

0.7 0.69 0.69 

0.8 0.81 0.81 

4.8 11 12 

XXXll xxxvm 

12 

10.3 

0.4 

0.2 

0.7 

0.8 

7.9 

NIST3=a+b•NIST1 

a:O 

b: 0.96 ±0.03 

R2: 0.974 

Serum 202 223 <--Previous Results--> 

DD 

MedianD 

eSDD 

n. 

Median. 

eSD. 

P(n=p) 

P(n<p) 

42 

17.8 

l.S 

227 

4S 

17.0 

1.4 

0.90 

0.61 

SD...,. 1.1 

cv...,. 6.S 

44 

7.72 

0.46 

RRXXXIX 

228 

46 

1.S4 

o.ss 

0.94 

0.14 

0 

0 

229 230 

46 46 

7.11 11.4 

0.74 1.2 

0 0.8 

0 7.3 

<-Current Results -> 

NAV 17.2 7.61 6.9S 10.8 <-Assignments-> 

NAU 1.4 0.81 0.81 1.2 

CV 8.1 11 12 11 

xCV 7.4 7.7 8.0 7.2 

(39 _dll)NlSTl:lt 

12 

3.51 

0.08 

0.11 

0.10 

0.17 

4.8 

XXXJJ 

202 

18 

3.76 

0.39 

227 

2S 

3.86 

0.25 

0.93 

0.98 

0.19 

4.9 

NIST 

12 12 12 

1.62 4.13 1.21 

0.06 0.17 0.03 

0.02 0.09 0.07 

0.10 0.10 0.10 

0.12 0.22 0.12 

7.1 S.3 10 

xxxvw 

223 

22 

1.68 

0.13 

RRXXXIX 

228 229 230 

2S 25 2S 

1.78 4.36 1.36 

0.09 0.30 0.14 

0.78 

0.96 

0 0.21 0.07 

0 4.7 S.3 

3.68 1.70 4.24 1.28 

0.2S 0.12 0.30 0.14 

6.9 6.8 7.1 11 

1.S 9.1 7.4 10 

NIST3=a+b•NIST1 

a:O 

b: 0.92 ±0.02 

R2: 0.988 

B10
 
Analysis Results 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean, 

so. 

SD...,. 

so .... SI>msr. 

CVNIST• 

·n 

Mean 

SD..., 

SD11e1 

SD""' 

s~ 

CVNIST 

RR 

Serum 

no 

Median0 

eSD0 

n. 

Median. 

eSD. 

P(n=p) 

P(n<p) 

so .... cv* 

227 

0 

0 

XXXll 

202 

1.0 

227 

4 

0.2 

0.0 

Round Robin XXXIX: Sera 227-230 7 

Table 1 

NIST Data and Value/Uncertainty Assignments 

8-Tocopherol Total p-Carotene 

NISTl NIST3 NISTl NIST3 

228 229 230 227 228 

0 0 0 0 0 

NIST 

0 6 6 

0.5 0.2 

0.1 0.0 

0.1 0.0 

lCXXVUl 

229 230 227 228 229 230 227 228 229 230 

0.6 0.3 1.22 0.179 0.112 0.110 1.14 0.143 0.076 0.079 

0.5 0.2 1.31 0.181 0.114 0.105 1.19 0.146 0.087 0.079 

0.5 0.2 1.27 0.182 0.114 0.114 1.17 0.145 0.078 0.074 

0.4 0.2 1.34 0.178 0.113 1.22 0.143 0.082 0.072 

0.5 0.2 1.30 0.171 0.111 0.110 1.22 0.144 0.080 0.073 

0.4 0.2 1.18 0.180 0.109 0.116 1.21 0.142 0.083 0.083 

6 6 6 6 6 5 6 6 6 6 

0.5 0.2 1.27 0.179 0.112 0.111 1.19 0.144 0.081 0.077 

0.1 0.0 0.06 0.004 0.002 0.004 0.03 0.002 0.004 0.004 

0.1 0.0 0.07 0.004 0.001 0.003 0.03 0.002 0.005 0.004 

0.1 0.0 0.03 0.003 0.002 0.004 0.02 0.001 0.001 0.003 

0.1 0.0 0.08 0.005 0.002 0.005 0.03 0.002 0.005 0.005 

22 18 5.9 2.7 1.9 4.3 2.9 1.5 6.2 6.8 

NIST 

12 12 12 11 

1.23 0.161 0.097 0.094 

0.05 0.003 0.004 0.002 

0.03 0.002 0.001 0.004 

0.00 0.001 0.001 0.001 

0.06 0.004 0.004 0.004 

4.7 2.3 4.1 4.6 

xxxu xxxvw 

NIST3=a+b*NIST1 

a: -0.027 ±0.001 

b: 0.961 ±0.001 

R2: 1.000 

223 <--Previous Results--> 202 223 

5 

0.17 

0.03 

RRXXXIX 

228 229 230 <-Current Results-> 

4 4 4 

0.15 0.5 0.4 

0.03 0.1 0.1 

0.63 

0.56 

32 31 

1.23 0.166 

0.20 0.017 

RRXXXIX 

227 228 229 

33 33 32 

1.24 0.177 0.111 

0.13 0.027 0.014 

0.99 0.90 

0.99 0.01• 

0.12 0.026 0.014 

9.6 15 12 

230 

33 

0.106 

0.017 

0.016 

15 

~~~l~~~~~~o-.5~-o-.3-' <-Assignments-> 1.24 0.169 0.104 0.100 

0.13 0.027 0.014 0.017 

CV 

xCV 

(39 _dlllNJSTm 

11 16 

12 19 

14 17 

21 22 

B11
 
Analysis Results Round Robin XXXIX: Sera 227-230 8 

Table 1 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

8:2 

C:l 

C:2 

n, 

Mean, 

so. 

SD...,, 

so ..... 

227 

1.076 

1.174 

1.127 

1.109 

1.083 

l.07S 

6 

1.107 

0.039 

0.041 

0.02S 

trans-p..Carotene 

NISTl NIST3 

228 229 230 227 228 229 

0.167 0.109 0.099 1.063 0.143 0.076 

0.173 0.104 0.090 1.108 0.146 0.087 

0.166 0.103 O.lOS 1.101 0.14S 0.078 

0.161 0.104 1.149 0.143 0.082 

0.162 0.102 0.106 1.IOS 0.144 0.080 

0.169 0.100 O.llS 1.101 0.142 0.083 

6 6 s 6 6 6 

0.166 0.104 0.103 1.104 0.144 0.081 

0.004 0.003 0.009 0.027 0.002 0.004 

0.004 0.002 o.oos 0.027 0.002 o.oos 

0.003 0.003 0.008 0.020 0.001 0.001 

Total a-Carotene 

NIST I NIST3 

230 227 228 229 230 227 228 229 230 

0.079 O.OS4 0.104 O.OS1 0.026 0.017 0.101 

0.079 O.OS2 0.086 0.060 0.024 0.020 0.097 

0.074 0.047 0.09S 0.054 0.02S 0.017 0.101 

0.072 0.042 0.061 0.02S 0.017 0.102 

0.073 0.04S 0.084 o.oss 0.023 0.016 0.105 

0.083 0.049 0.111 O.OS1 0.022 0.014 0.117 

6 6 0 0 5 6 6 6 6 

0.077 0.048 0.096 0.057 0.024 0.017 0.104 

0.004 o.oos 0.011 0.003 0.001 0.002 0.007 

0.004 0.003 0.013 0.003 0.001 0.001 0.005 

0.003 0.004 0.001 0.001 0.001 0.002 0.006 

SI>msr1 0.048 O.OOS 0.003 0.010 0.033 0.002 O.OOS 0.005 O.OOS 

CVNISTI 4.3 3.3 3.3 9.3 3.0 l.S 6.2 6.8 11 

0.013 0.004 0.002 0.002 0.008 

14 6.3 6.3 12 7.7 

n 

Mean 

SD..., 

so .... SD1111 

12 

1.106 

0.037 

0.020 

0.001 

NIST 

12 12 11 

O.ISS 0.092 0.090 

0.003 0.004 0.004 

0.002 0.002 0.006 

0.001 0.001 0.001 

SI>msr 0.043 0.004 0.004 0.007 

CVNIST 3.8 2.7 4.7 7.9 

RR XXXD XXXVID 

NIST3=a+b•NIST1 

a: -0.025 ±0.001 

b: 1.020±0.001 

R2: 1.000 

Serum 202 223 <--Previous Results--> 

n, 

Median, 

eSD, 

no 

Median, 

eSD. 

P(n=p) 

P(n<p) 

8 

1.108 

0.070 

227 

11 

1.164 

0.064 

0.70 

0.63 

12 

0.161 

0.020 

RRXXXIX 

228 229 230 

11 11 11 

O.ISO 0.097 0.096 

0.019 0.010 0.020 

0.82 

0.61 

SD18 0.048 0.018 0.009 0.019 

cv...,. 4.1 12 8.8 20 

NAV 1.13S 0.153 0.09S 0.093 

NAu.o_._064;..;...._o~0-19 __ 0_.0_10;;........;;o_.02,__,o 

CV S.6 12 10 22 

xCV 9.0 9.8 11 11 

(39 _dll)NISTW 

<-Current Results -> 

<-Assignments-> 

NIST 

12 6 6 11 

O.OS3 0.024 0.017 0.100 

0.004 0.001 0.001 0.009 

0.001 0.001 0.002 0.006 

0.003 0.003 0.003 0.003 

0.005 0.004 0.004 0.012 

9.6 lS 22 12 

XXXll xxxvm 

202 223 

21 25 

0.039 0.026 

O.ot6 0.009 

RRXXXIX 

227 228 229 230 

27 27 27 28 

0.045 0.027 0.020 0.141 

0.014 O.ot5 0.012 0.033 

0.91 0.98 

0.76 0.01* 

0.013 0.014 0.011 0.031 

28 S3 SS 22 

0.049 0.026 

0.014 0.015 

28 S8 

28 30 

0.018 

0.012 

63 

33 

0.120 

0.033 

28 

26 

NIST3=a+b•Median 

a: -0.018 ±0.006 

b: 1.664 ±0.176 

R2: 0.978 

B12
 
Analysis Results Round Robin XXXIX: Sera 227- 230 9 

Table 1 

NIST Data and Value/Uncertainty Assignments 

trans-ex-Carotene Total Lycopene 

NIST I NIST3 NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean1 

so. 

SOreo• 

so ... 

227 228 229 

0 0 

230 227 

0.03 

0.04 

0.03 

0.04 

0.03 

0.03 

0 0 6 

0.03 

0.00 

0.00 

0.00 

228 229 230 

0.03 0.017 0.10 

0.02 0.020 0.10 

0.02 0.017 0.10 

0.02 0.017 0.10 

0.02 0.016 0.11 

0.02 0.014 0.12 

6 6 6 

0.02 0.017 0.10 

0.00 0.002 0.01 

0.00 0.001 0.00 

0.00 0.002 O.ot 

227 228 229 230 227 228 229 230 

0.298 0.454 0.56 0.360 

0.335 0.443 0.57 0.389 

0.340 0.448 0.57 0.358 

0.340 0.488 0.58 0.358 

0.337 0.474 0.57 0.345 

0.300 0.454 0.52 0.400 

0 0 0 0 6 6 6 6 

0.325 0.460 0.56 0.368 

0.020 0.017 0.02 0.021 

0.021 0.019 0.02 0.025 

0.013 0.010 O.ot 0.009 

SDmsr. 

cvNIST. 

0.00 0.00 0.002 O.ot 0.025 0.021 0.03 0.027 

10 6.3 12 7.7 7.7 4.7 4.5 7.3 

NIST NIST NIST3=a+b*Median 

' n 

Mean 

SDreo 

SD"" 

so. 

SDmsr 

CVNIST 

6 6 

0.03 0.02 

0.00 0.00 

0.00 0.00 

RR XXXD xxxvm 

Seruml::J02 223 

Do 0 0 

Median, 

eSD0 

6 6 

0.017 0.10 

0.001 0.00 

0.002 0.01 

<--Previous Results--> 

RRXXXIX 

n. 

Median. 

eso. 

P(n=p) 

P(n<p) 

SD11111 

CV11111 

227 228 

0 

229 230 <-Current Results -> 

0 0 0 

6 6 6 6 

0.325 0.460 0.56 0.368 

O.ot5 0.024 O.ot 0.012 

0.013 0.010 O.ot 0.009 

0.010 0.010 O.ot 0.010 

0.022 0.028 0.02 0.018 

6.8 6.0 3.2 4.9 

XXXll xxxvw 

202 223 

22 27 

0.314 0.463 

0.068 0.084 

RRXXXIX 

227 228 229 

27 27 26 

0.328 0.470 0.60 

0.060 0.108 0.15 

0.95 0.98 

0.74 0.10 

230 

27 

0.421 

0.097 

0.056 0.105 0.15 0.095 

17 22 24 23 

~~~ 1 .... _o_.0_3_0_.0_2_0_.0_11 __ 0._10 ... 1 <-Assignments-> ... ~=:060 =32 .... 6-~=.... 46 10--~-~ ... :~ ..... :_o __ _~-~ CV 18 23 25 25 

~ ~ n n ~ 

(39_dalNIS'l'm 

a: 0.044 ±0.025 

b: 0.869 ±0.051 

R2: 0.993 

B13
 
Analysis Results Round Robin XXXIX: Sera 227-230 10 

Table 1 

NIST Data and Value/Uncertainty Assignments 

trans-Lycopene 

NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean, 

so. 

so_ 

so .... s0msr. 

CVNISTI 

n 

Mean 

SOieo 

so .... so .. 

227 

0 

6 

0.150 

0.006 

0.005 

0.003 

228 229 230 

0 0 0 

NIST 

6 6 6 

0.190 0.347 0.183 

0.004 0.007 0.005 

0.004 0.007 0.006 

0.003 0.003 0.003 

SDmsr 0.008 0.006 0.010 0.008 

CVNIST 5.3 3.4 2.9 4.5 

RR XXXD xxxvm 

227 228 229 230 

0.138 0.183 0.333 0.179 

0.151 0.189 0.349 0.188 

0.155 0.191 0.352 0.179 

0.153 0.197 0.356 0.175 

0.151 0.191 0.364 0.179 

0.151 0.188 0.328 0.199 

6 6 6 6 

0.150 0.190 0.347 0.183 

0.006 0.005 0.014 0.009 

0.006 0.004 0.016 0.009 

0.005 0.004 0.007 0.006 

0.007 0.005 O.Ql8 O.ot 1 

4.9 2.9 5.1 6.1 

NIST3=a+b*Median 

a: 0.034 ±0.004 

b: 0.632 ±0.012 

R2: 0.999 

Serum 202 223 <--Previous Results--> 

no 

Median0 

eS00 

n,, 

Median. 

eS00 

P(n=p) 

P(n<p) 

0.178 

227 

8 

0.181 

0.024 

8 

0.251 

0.042 

RRXXXIX 

228 229 230 

8 8 8 

0.250 0.494 0.290 

0.029 0.038 0.044 

0.99 

0.83 

S011111 0.023 0.028 0.037 0.043 

CV11111 13 11 7.4 15 

<-Current Results -> 

NA V 0.165 0.220 0.420 0.236 <-Assignments-> 

NAU 0.024 0.029 0.038 0.044 

CV 15 13 9.0 19 

xCV 

13-Cryptoxanthin 

NISTl NIST3 

227 228 229 230 

0 0 0 0 

NIST 

6 6 6 6 

0.032 0.039 0.038 0.054 

0.002 0.003 0.001 0.003 

0.001 0.003 0.003 0.001 

0.001 0.001 0.001 0.001 

0.002 0.004 0.003 0.003 

6.9 11 7.6 6.2 

XXX1I xxxvw 

202 223 

16 19 

0.049 0.055 

0.016 0.014 

RRXXXIX 

227 228 229 230 

24 24 24 24 

0.037 0.055 0.056 0.076 

0.012 0.014 O.ot5 0.019 

0.79 1.00 

0.90 0.46 

0.012 0.014 0.014 0.019 

31 25 26 25 

0.034 0.047 0.047 0.065 

0.012 0.014 O.ot5 0.019 

34 31 31 29 

30 28 28 26 

227 228 229 230 

0.032 0.040 0.042 0.054 

0.030 0.035 0.041 0.054 

0.031 0.044 0.036 0.058 

0.034 0.041 0.036 0.053 

0.031 0.036 0.039 0.052 

0.032 0.038 0.036 0.056 

6 6 6 6 

0.032 0.039 0.038 0.054 

0.001 0.003 0.003 0.002 

0.002 0.003 0.001 0.003 

0.001 0.003 0.003 0.001 

0.002 0.004 0.003 0.003 

5.6 10 7.9 5.5 

NIST3=a+b*Mcdian 

a: 0.017 ±0.002 

b: 0.396 ±0.040 

R2: 0.980 

B14
 
Analysis Results Round Robin XXXIX: Sera 227-230 II 

Table 1 

NIST Data and Value/Uncertainty Assignments 

"Lutein" "Zeaxanthin" 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean, 

so. 

so..,OI 

SObeb 

s0wr. 

cvNJST. 

n 

Mean 

so ... so. 

so .. 

227 

0 

6 

0.045 

0.002 

0.002 

0.006 

NISTl 

228 229 230 

0 0 0 

NIST 

6 6 6 

0.118 0.13 0.676 

0.004 0.00 0.010 

0.001 0.00 O.ot 1 

0.006 0.01 0.006 

Sl>wr 0.007 0.007 O.ot 0.016 

CVNIST 15 6.1 5.3 2.4 

RR XXXD xxxvm 

NIST3 

227 228 229 230 

0.046 0.123 0.13 0.676 

0.046 0.116 0.13 0.683 

0.045 0.121 0.13 0.671 

0.041 0.117 0.13 0.655 

0.045 0.116 0.13 0.674 

0.048 0.118 0.13 0.694 

6 6 6 6 

0.045 0.118 0.13 0.676 

0.002 0.003 0.00 0.013 

0.002 0.003 0.00 0.011 

0.002 0.001 0.00 O.ot 1 

0.002 0.004 0.00 0.016 

5.4 3.0 2.5 2.3 

NIST3=a+b*Median 

a: 0.015 ±0.008 

b: 0.847 ±0.080 

R2: 0.983 

Serum 202 223 <--Previous Results--> 

n, 

Median, 

eSO, 

n. 

Median. 

eS01 

P(n=p) 

P(n<p) 

11 14 

0.036 0.125 

o.oi5 0.010 

RRXXXIX 

227 228 229 

12 12 11 

0.037 0.116 0.14 

0.009 0.017 0.28 

0.99 0.81 

0.94 0.06 

230 

11 

0.788 

0.082 

so...,. 0.006 0.015 0.28 0.080 

cv...,. 17 13 200 10 

<-Current Results-> 

NAV 0.041 0.117 0.13 0.732 <-Assignments-> 

NAU 0.009 0.017 0.28 0.082 

CV 22 14 210 11 

xCV 

(39_dllJNISTIJll 

NISTl 

227 228 229 230 

0 0 0 0 

NIST 

6 6 6 6 

0.023 0.027 0.75 0.078 

0.002 0.006 O.ot 0.004 

0.001 0.003 0.01 0.003 

0.009 0.009 O.ot 0.009 

0.009 O.ot 1 O.ot 0.010 

39 41 1.7 13 

XXXD XXXVIU 

202 223 

6 11 

0.014 0.029 

0.012 0.010 

RRXXXIX 

227 228 229 230 

9 10 9 9 

0.014 0.037 0.77 0.087 

0.006 O.ot8 0.13 0.018 

1.00 0.82 

0.96 0.04• 

o 0.014 0.13 o.oi5 

0 38 17 17 

0.018 0.032 0.76 0.082 

0.009 O.ot8 0.13 O.ot8 

48 56 18 22 

NIST3 

227 228 229 230 

0.023 0.034 0.74 0.081 

0.024 0.02S 0.76 0.079 

0.023 0.024 0.74 0.078 

0.021 0.033 0.74 0.071 

0.023 0.019 0.75 0.076 

0.024 0.029 0.73 0.081 

6 6 6 6 

0.023 0.027 0.75 0.o78 

0.001 0.006 o.oi 0.004 

0.001 0.007 o.oi 0.004 

0.001 0.003 0.01 0.003 

0.001 0.007 O.ot 0.004 

6.4 27 1.6 5.6 

NIST3=a+b*Median 

a:O 

b: 0.973 ±0.011 

R2: 0.999 

B15
 
Analysis of Results 

Round Robin XXXIX:Sera:227-230 

Table 2 

Summary of NIST Assigned V aloes & Uncertainties 

227 228 229 2

Analyte NAV NAU CV NAV NAU CV NAV NAU CV NAV 

Retinol 0.869 0.056 6 0.488 0.032 7 0.377 0.036 9 0.665 0

Retinyl Palmitate 0.228 0.024 11 0.065 0.039 59 0.098 0.028 28 0.172 0

a-Tocopherol 17.2 1.4 8 7.61 0.81 11 6.95 0.81 12 10.8 1

y-Tocopherol 3.68 0.25 7 1.70 0.12 7 4.24 0.30 7 1.28 0

8-Tocopherol 0.5 0.3 

Total p-Carotene 1.24 0.13 11 0.169 0.027 16 0.104 0.014 14 0.100 0

trans-p-Carotene 1.135 0.064 6 0.153 0.019 12 0.095 0.010 10 0.093 0

Total a-Carotene 0.049 0.014 28 0.026 0.015 58 0.018 0.012 63 0.120 0

trans-a-Carotene 0.03 0.02 0.017 0.10 

Total Lycopene 0.326 0.060 18 0.465 0.108 23 0.58 0.15 25 0.395 0

trans-Lycopene 0.165 0 . 024 15 0 . 220 0.029 13 0.420 0.038 9 0.236 0

p-Cryptoxanthin 0.034 0.012 34 0.047 0.014 31 0.047 0.015 31 0.065 0

"Lutein" 0.041 0.009 22 0.117 0.017 14 0.13 0.28 210 0.732 0

"Zeaxanthin" 0.018 0.009 48 0.032 0.018 56 0.76 0.13 18 0.082 0

ll9_doljSummaryTu 

B16
 

 

Appendix C. “All-Lab Report” for RR39 

The following 6 pages are the “All-Lab Report” as provided to all participants, with two 

exceptions: 

• the participant identifiers (Lab) have been altered. 

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

The data summary in the “All-Lab Report” has been altered to ensure confidentiality of 

identification codes assigned to laboratories. 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. 

C1
 
Round Robin XXXIX Laboratory Results 

Values in μg/mL 

Retinol Retinyl Palmitate α-Tocopherol γ-Tocopherol δ-Tocopherol 

Lab 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BGa 

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-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 

FSV-CH 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CT 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DJ 

FSV-DL 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DS 

FSV-DU 

FSV-EI 

FSV-EL 

FSV-EM 

FSV-FN 

227 228 229 230 

0.853 0.502 0.406 0.707 

227 228 229 230 227 228 229 230 227 228 229 230 227 228 229 230 

0.243 0.104 0.095 0.161 17.4 7.92 7.28 11.4 3.86 1.92 4.44 1.51 

0.830 0.478 0.361 0.662 16.6 7.50 7.00 10.9 

0.925 0.531 0.388 0.752 17.7 7.99 7.92 12.7 3.74 1.71 4.65 1.32 

0.880 0.530 0.430 0.780 17.6 7.80 7.30 12.1 3.60 1.70 4.10 1.30 

0.997 0.555 0.439 0.799 0.236 0.079 0.121 0.195 17.8 8.04 7.79 12.5 3.89 1.78 4.74 1.37 

1.042 0.598 0.523 0.932 0.258 0.092 0.141 0.244 18.5 8.41 8.04 13.1 3.82 1.79 4.59 1.34 

0.875 0.497 0.333 0.677 0.253 0.037 0.116 0.223 17.5 8.00 7.31 11.5 3.73 1.76 4.31 1.28 

0.837 0.493 0.393 0.680 0.299 0.204 0.128 0.282 18.1 7.95 7.09 11.7 4.01 1.81 4.24 1.36 

0.864 0.521 0.387 0.719 0.234 0.078 0.144 0.189 16.0 7.79 7.11 11.8 3.73 1.81 4.50 1.45 

0.858 0.483 0.384 0.687 19.5 8.72 7.83 12.8 

0.487 0.372 0.687 5.17 6.46 10.3 

0.859 0.520 0.497 0.696 17.7 7.10 6.50 10.0 

0.820 0.470 0.370 0.710 0.230 0.060 0.100 0.230 16.3 7.32 6.99 11.5 3.96 1.86 4.74 1.36 0.220 0.21 0.56 0.46 

0.805 0.444 0.329 0.602 15.9 7.15 6.46 10.4 

0.859 0.470 0.397 0.670 18.8 7.78 6.65 11.5 

0.740 0.550 0.390 0.680 

0.910 0.560 0.390 0.690 

0.880 0.420 0.310 0.620 

17.6 7.44 6.95 9.8 

0.899 0.483 0.405 0.788 0.240 0.095 0.122 0.262 17.9 8.25 7.78 11.4 4.18 1.83 4.64 1.43 0.218 0.13 0.75 0.46 

0.846 0.441 0.357 0.514 14.1 5.83 5.68 7.3 3.33 1.52 3.82 1.02 

0.828 0.483 0.355 0.678 15.9 7.32 6.62 11.5 4.00 1.86 4.83 1.44 

0.930 0.510 0.420 0.670 0.230 0.047 0.068 0.126 18.1 7.80 7.01 11.3 4.03 1.78 4.66 1.30 

1.006 0.510 0.425 0.765 17.8 7.19 7.47 11.0 3.90 1.81 4.28 1.59 

0.887 0.514 0.387 0.678 0.272 0.125 0.130 0.181 17.5 7.92 6.88 10.3 3.76 1.73 4.36 1.19 0.152 0.16 0.42 0.22 

15.8 7.17 8.20 10.6 4.50 1.70 4.35 3.80 

0.737 0.474 !0.302 !0.603 13.8 5.89 !4.32 !7.93 

0.760 0.430 0.300 0.580 18.1 7.88 7.47 11.3 

0.850 0.492 0.355 0.603 15.1 6.17 5.67 9.3 

0.772 0.501 0.419 0.723 0.318 0.110 0.098 0.082 18.8 9.05 7.55 11.6 3.55 1.82 4.79 1.42 

0.873 0.497 0.383 0.683 17.9 7.87 6.91 11.5 

0.855 0.489 0.361 0.620 17.3 7.50 7.10 11.9 

0.906 0.588 0.549 0.840 11.8 3.81 3.22 6.9 4.01 2.03 4.47 1.61 

0.838 0.481 0.382 0.682 16.6 7.19 6.27 11.1 3.42 1.56 3.92 1.17 

0.884 0.471 0.394 0.741 16.7 7.36 6.88 11.2 3.50 1.64 4.08 1.35 

1.131 0.587 0.285 0.819 16.9 7.05 6.47 11.0 3.07 1.74 3.34 1.58 

17.9 7.39 8.01 10.4 

0.837 0.500 0.411 0.722 16.7 7.29 7.21 11.9 3.40 1.44 4.25 1.11 

17.2 8.22 7.51 12.1 3.64 1.72 4.17 1.52 

0.718 0.507 0.349 0.696 16.3 7.93 7.54 12.1 

0.886 0.513 0.387 0.699 

0.920 0.480 0.380 0.700 

18.6 8.20 7.68 12.3 7.06 3.23 8.32 2.25 0.103 nd 0.27 nd 

0.908 0.486 0.375 0.537 15.5 8.06 7.26 11.4 

0.831 0.492 0.402 0.724 0.262 0.127 0.080 0.111 16.7 7.26 6.25 9.9 

0.870 0.510 0.380 0.670 0.120 0.010 0.060 0.190 17.3 8.65 8.15 12.3 4.03 1.70 4.72 1.49 

0.889 0.486 0.380 0.705 0.234 0.049 0.077 0.160 17.0 7.68 7.06 11.3 4.03 1.78 4.75 1.37 0.183 0.14 0.49 0.28 

0.920 0.530 0.280 0.690 16.9 7.83 6.08 11.7 

0.550 0.410 0.310 0.680 11.1 6.10 7.60 12.1 

0.848 0.477 0.384 0.643 

0.932 0.525 0.398 0.728 

17.8 8.03 7.64 11.7 3.87 1.93 4.58 1.49 

0.820 0.440 0.360 0.690 18.6 9.47 8.43 14.3 4.03 1.88 4.28 1.63 

0.851 0.459 0.354 0.673 16.6 7.50 7.29 11.9 

0.990 0.500 0.330 0.550 15.3 7.62 7.23 10.2 

1.243 0.478 0.417 0.908 23.2 7.57 8.06 12.7 

0.763 0.404 0.310 0.527 

0.930 0.520 0.430 0.760 

14.8 6.54 6.25 10.3 3.67 1.71 4.12 1.31 

0.850 0.540 0.320 0.660 14.7 6.40 4.20 7.7 

0.891 0.515 0.382 0.693 18.8 8.35 7.26 12.0 3.76 1.81 4.13 1.36 

n 53 54 53 53 14 14 14 14 51 52 51 51 30 30 30 30 5 4 5 4 

Min 0.550 0.404 0.280 0.514 0.120 0.010 0.060 0.082 11.1 3.81 3.22 6.9 3.07 1.44 3.34 1.02 0.103 0.133 0.27 0.220 

Median 0.864 0.495 0.383 0.690 0.241 0.086 0.108 0.190 17.3 7.65 7.21 11.5 3.84 1.78 4.40 1.37 0.183 0.149 0.49 0.368 

Max 1.243 0.598 0.549 0.932 0.318 0.204 0.144 0.282 23.2 9.47 8.43 14.3 7.06 3.23 8.32 3.80 0.220 0.210 0.75 0.465 

eSD 0.052 0.029 0.034 0.043 0.017 0.046 0.031 0.055 1.1 0.57 0.64 0.9 0.27 0.11 0.38 0.12 0.052 0.11 

eCV 6 6 9 6 7 54 29 29 7 7 9 8 7 6 9 9 29 23 

NISTa
 

NISTb
 

NAV 

NAU 

0.889 0.494 0.388 0.657 0.248 nq nq nq 17.5 8.19 7.21 10.5 3.59 1.68 4.34 1.32 

0.870 0.476 0.354 0.628 0.181 0.045 0.078 0.152 17.3 7.19 6.35 10.1 3.43 1.55 3.92 1.10 nd nd 0.48 0.22 

0.872 0.490 0.377 0.666 0.241 0.086 0.108 0.190 17.4 7.67 7.00 10.9 3.67 1.70 4.26 1.29 0.48 

0.074 0.042 0.036 0.066 0.017 0.046 0.031 0.055 1.4 0.75 0.76 1.4 0.43 0.23 0.45 0.20 0.11 

All Lab Report C2 Page 1 / 6 
Round Robin XXXIX Laboratory Results 

Values in μg/mL 

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

Lab 227 228 229 230 227 228 229 230 227 228 229 230 227 228 229 230 

FSV-BA 1.22 0.181 0.119 0.131 1.17 0.172 0.112 0.123 0.058 0.009 0.007 0.008 0.056 0.035 0.028 0.155 

FSV-BD 0.90 0.126 0.094 0.098
 

FSV-BE
 1.29 0.188 0.119 0.099
 

FSV-BF
 1.17 0.139 0.083 0.063 0.065 0.018 0.016 0.157 

FSV-BG 1.19 0.185 0.111 0.112 0.045 0.025 0.020 0.135 

FSV-BGa 1.23 0.180 0.111 0.114 0.051 0.048 0.039 0.120 

FSV-BH 1.28 0.175 0.103 0.115 1.21 0.169 0.101 0.109 0.075 nd nd nd 0.048 0.026 0.018 0.179 

FSV-BI 1.34 0.176 0.104 0.117 0.043 0.027 0.018 0.145 

FSV-BJ 1.35 0.196 0.119 0.116 0.057 0.038 0.027 0.159 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 1.28 0.160 0.110 0.110 1.20 0.150 0.097 0.101 0.080 0.010 0.013 0.009 0.040 0.020 0.015 0.170 

FSV-BO 0.90 0.165 0.082 0.080 0.037 0.020 0.014 0.053 

FSV-BP 1.18 0.101 0.093 0.102 0.042 0.013 0.014 0.097 

FSV-BQ 

FSV-BR 

FSV-BS 1.24 0.200 0.120 0.120 1.18 0.170 0.120 0.120 0.055 0.032 nd nd 0.059 0.047 0.038 0.133 

FSV-BT 1.24 0.178 0.113 0.119 1.16 0.172 0.107 0.113 0.083 0.006 0.006 0.006 0.035 0.034 0.026 0.206 

FSV-BU 1.12 0.146 0.100 0.101 0.031 0.016 0.013 0.095 

FSV-BV 1.01 0.164 0.117 0.103 0.029 0.017 0.012 0.121 

FSV-BW 1.40 0.211 0.112 0.103 0.027 0.027 0.016 0.107 

FSV-BX 1.41 0.330 0.274 0.083 0.040 0.038 0.156 

FSV-BY 1.28 0.177 0.100 0.092 1.16 0.165 0.090 0.084 0.117 0.012 0.011 0.008 0.050 0.040 0.029 0.092 

FSV-BZ 0.90 0.140 0.080 0.083 nq nd nd nd 0.070 0.050 0.033 0.102 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 0.88 0.090 0.050 0.034 0.028 0.012 0.010 0.043 

FSV-CE 1.10 0.172 0.107 0.138
 

FSV-CF
 

FSV-CG
 1.52 0.216 0.137 0.142 0.055 0.040 0.033 0.156 

FSV-CH 1.21 0.163 0.101 0.091 0.026 0.019 0.010 0.152 

FSV-CK 1.22 0.188 0.134 0.147 0.055 0.045 0.038 0.178 

FSV-CL 1.56 0.167 0.086 0.097 0.049 0.023 0.011 0.144 

FSV-CM 

FSV-CN 0.53 0.073 0.039 0.051 nd nd nd 0.080 

FSV-CP 1.14 0.145 0.102 0.104 0.036 0.018 0.014 0.129 

FSV-CQ 1.78 0.239 0.075 0.052
 

FSV-CR
 

FSV-CS
 1.29 0.159 0.102 0.098 1.16 0.145 0.092 0.088 0.131 0.014 0.010 0.010 0.052 0.026 0.016 0.144 

FSV-CT 1.01 0.085 0.052 0.067
 

FSV-CU
 

FSV-CX
 1.48 0.210 0.160 0.140 0.040 0.020 0.010 0.100 

FSV-DA 1.13 0.156 0.116 0.106 1.04 0.144 0.101 0.096 0.090 0.012 0.015 0.010 0.045 0.021 0.017 0.138 

FSV-DB 1.16 0.150 0.060 0.080
 

FSV-DJ
 

FSV-DL
 1.47 0.192 0.120 0.126 0.054 0.033 0.024 0.145 

FSV-DP 

FSV-DQ 1.30 0.224 0.141 0.135 0.043 0.084 0.053 0.350 

FSV-DR 1.44 0.185 0.149 0.084
 

FSV-DS
 0.17 0.230 0.350 0.210
 

FSV-DU
 1.68 0.152 0.125 0.140
 

FSV-EI
 1.19 0.150 0.092 0.083 0.036 0.028 0.020 0.113 

FSV-EL
 

FSV-EM
 

FSV-FN
 

n 37 37 36 37 11 11 11 11 8 7 6 6 30 30 30 31 

Min 0.17 0.085 0.050 0.034 0.53 0.073 0.039 0.051 0.055 0.006 0.006 0.006 0.026 0.012 0.010 0.043 

Median 1.24 0.176 0.111 0.106 1.16 0.150 0.097 0.096 0.082 0.012 0.011 0.009 0.045 0.027 0.018 0.138 

Max 1.78 0.330 0.350 0.274 1.21 0.172 0.120 0.123 0.131 0.032 0.015 0.010 0.083 0.084 0.053 0.350 

eSD 0.16 0.030 0.015 0.021 0.06 0.022 0.010 0.019 0.024 0.003 0.005 0.001 0.014 0.013 0.010 0.031 

eCV 13 17 13 20 5 15 10 20 29 25 44 17 30 47 54 23 

NISTa 

NISTb 

NAV 

NAU 

1.27 0.179 0.112 0.111 1.11 0.166 0.104 0.103 0.162 0.012 0.009 0.008 0.048 nq nq 0.096 

1.19 >0.144 >0.081 >0.077 1.10 0.144 0.081 0.077 0.087 nq nq nq 0.057 0.024 0.017 0.104 

1.24 0.169 0.104 0.100 1.13 0.153 0.095 0.093 0.103 0.012 0.010 0.008 0.049 0.025 0.017 0.119 

0.16 0.031 0.023 0.023 0.12 0.019 0.017 0.021 0.078 0.005 0.005 0.006 0.015 0.015 0.011 0.047 

All Lab Report C3 Page 2 / 6 
Round Robin XXXIX Laboratory Results 

Values in μg/mL 

Total Lycopene trans-Lycopene β-Cryptoxanthin α-Cryptoxanthin 

Lab 227 228 229 230 227 228 229 230 227 228 229 230 227 228 229 230 

FSV-BA 0.181 0.266 0.48 0.296 0.049 0.073 0.046 0.087
 

FSV-BD
 0.209 0.31 0.50 0.31 0.030 0.048 0.049 0.062
 

FSV-BE
 

FSV-BF
 0.379 0.54 0.75 0.55
 

FSV-BG
 0.328 0.53 0.74 0.48 0.162 0.249 0.47 0.266 0.029 0.054 0.050 0.075 

FSV-BGa 0.369 0.54 0.73 0.49
 

FSV-BH
 0.358 0.55 0.76 0.52 0.048 0.074 0.074 0.098
 

FSV-BI
 0.407 0.56 0.86 0.57 0.046 0.062 0.067 0.100
 

FSV-BJ
 0.317 0.44 0.74 0.46 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.340 0.49 0.80 0.54 0.180 0.250 0.58 0.310 0.030 0.040 0.050 0.070 0.010 0.010 0.030 0.030 

FSV-BO 0.357 0.50 0.57 0.45 0.027 0.044 0.050 0.069
 

FSV-BP
 0.263 0.09 0.45 0.33 0.077 0.117 0.045 0.062
 

FSV-BQ
 

FSV-BR
 

FSV-BS
 0.270 0.38 0.52 0.35 0.021 0.035 0.038 0.053
 

FSV-BT
 0.306 0.45 0.59 0.42 0.248 0.361 0.52 0.359 0.046 0.067 0.070 0.096 0.017 0.029 0.046 0.041 

FSV-BU 0.320 0.38 0.54 0.45 0.042 0.079 0.103 0.100
 

FSV-BV
 0.243 0.34 0.49 0.30 0.011 0.019 0.019 0.026 

FSV-BW 0.300 0.47 0.59 0.39
 

FSV-BX
 0.389 0.29 0.20 0.016 0.029 0.031 0.044 

FSV-BY 0.326 0.50 0.61 0.38 0.181 0.237 0.44 0.221 0.045 0.049 0.050 0.063
 

FSV-BZ
 0.300 0.300 0.51 0.325
 

FSV-CA
 

FSV-CB
 

FSV-CC
 

FSV-CD
 0.295 0.31 0.43 0.26 0.035 0.050 0.081 0.080
 

FSV-CE
 

FSV-CF
 

FSV-CG
 0.277 0.42 0.58 0.40 0.041 0.088 0.083 0.102
 

FSV-CH
 0.207 0.32 0.52 0.34
 

FSV-CK
 0.371 0.67 0.81 0.61 0.026 0.063 0.075 0.086 0.016 0.055 0.076 0.073 

FSV-CL 0.333 0.50 0.63 0.45 0.032 0.036 0.035 0.043 

FSV-CM 

FSV-CN 0.179 0.25 0.41 0.25 0.030 0.046 0.048 0.075
 

FSV-CP
 0.289 0.39 0.57 0.41 0.039 0.064 0.074 0.093
 

FSV-CQ
 

FSV-CR
 

FSV-CS
 0.343 0.50 0.65 0.42 0.035 0.053 0.058 0.072
 

FSV-CT
 

FSV-CU
 

FSV-CX
 0.250 0.36 0.56 0.35 0.060 0.100 0.100 0.140
 

FSV-DA
 0.330 0.48 0.74 0.50 0.166 0.231 0.51 0.283 0.039 0.055 0.068 0.083 0.010 0.018 0.040 0.039 

FSV-DB 0.382 0.52 0.64 0.41 0.054 0.066 0.057 0.095
 

FSV-DJ
 

FSV-DL
 0.340 0.46 0.56 0.39 0.036 0.055 0.068 0.077
 

FSV-DP
 

FSV-DQ
 0.374 0.61 0.85 0.53 0.039 0.065 0.068 0.081
 

FSV-DR
 

FSV-DS
 

FSV-DU
 

FSV-EI 0.135 0.173 0.34 0.150 0.032 0.047 0.054 0.073 

FSV-EL
 

FSV-EM
 

FSV-FN
 

n 30 30 29 30 8 8 8 8 27 27 27 27 4 4 4 4 

Min 0.179 0.09 0.41 0.20 0.135 0.173 0.34 0.150 0.011 0.019 0.019 0.026 0.010 0.010 0.030 0.030 

Median 0.327 0.46 0.59 0.42 0.181 0.250 0.49 0.290 0.036 0.055 0.057 0.077 0.013 0.024 0.043 0.040 

Max 0.407 0.67 0.86 0.61 0.300 0.361 0.58 0.359 0.077 0.117 0.103 0.140 0.017 0.055 0.076 0.073 

eSD 0.060 0.11 0.14 0.10 0.024 0.026 0.04 0.044 0.010 0.016 0.016 0.022 

eCV 18 24 24 25 14 10 7 15 29 30 29 29 

NISTa
 

NISTb
 

NAV 

NAU 

0.325 0.46 0.56 0.37 0.150 0.190 0.35 0.183 0.032 0.039 0.038 0.054 

0.326 0.46 0.58 0.39 

0.077 0.11 0.15 0.11 

0.165 0.220 0.42 0.236 

0.043 0.066 0.15 0.096 

0.034 0.047 0.048 0.066 

0.012 0.019 0.022 0.026 

All Lab Report C4 Page 3 / 6 
Round Robin XXXIX Laboratory Results 

Values in μg/mL 

Lutein Zeaxanthin Lutein&Zeaxanthin Total Carotenoids 

Lab 227 228 229 230 227 228 229 230 227 228 229 230 227 228 229 230 

FSV-BA 0.061 0.208 1.33 1.27
 

FSV-BD
 0.028 0.098 0.10 0.69 0.013 0.032 0.67 0.076 0.041 0.130 0.77 0.77 

FSV-BE 

FSV-BF 

FSV-BG
 0.050 0.136 0.18 0.89 0.009 0.028 0.95 0.068 0.059 0.164 1.13 0.96

FSV-BGa
 

FSV-BH
 0.027 0.103 0.09 0.74 nd 0.023 0.77 0.059 0.027 0.126 0.86 0.80 

FSV-BI 0.037 0.119 0.10 0.71 0.012 0.036 0.69 0.093 0.049 0.155 0.79 0.80 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.018 0.100 0.80 0.72 0.010 0.050 0.04 0.100 0.028 0.150 0.84 0.82 

FSV-BO 0.027 0.102 0.64 0.60
 

FSV-BP
 

FSV-BQ
 

FSV-BR
 

FSV-BS
 0.019 0.110 0.71 0.83
 

FSV-BT
 0.039 0.121 0.023 0.089 nd nd 0.061 0.160 0.84 0.83 1.846 1.130 1.923 1.967 

FSV-BU 0.037 0.139 0.74 0.72
 

FSV-BV
 0.040 0.127 0.65 0.60 

FSV-BW 

FSV-BX 0.045 0.137 0.14 0.91 0.014 0.034 0.83 0.077 0.059 0.171 0.96 0.99 

FSV-BY 0.037 0.126 1.02 0.82 0.020 0.037 0.06 0.136 0.057 0.163 1.11 1.09
 

FSV-BZ
 0.036 0.105 0.24 0.25
 

FSV-CA
 

FSV-CB
 

FSV-CC
 

FSV-CD
 0.068 0.227 1.34 1.12
 

FSV-CE
 

FSV-CF
 

FSV-CG
 0.076 0.232 0.98 0.98
 

FSV-CH
 

FSV-CK
 0.059 0.194 0.80 0.82
 

FSV-CL
 0.052 0.133 0.53 0.68 

FSV-CM 

FSV-CN 0.076 0.129 0.84 0.72
 

FSV-CP
 0.049 0.195 1.27 0.97
 

FSV-CQ
 

FSV-CR
 

FSV-CS
 0.052 0.151 0.77 0.82
 

FSV-CT
 

FSV-CU
 

FSV-CX
 0.040 0.210 0.19 0.55 0.010 0.040 0.41 0.100 0.050 0.250 0.60 0.65 

FSV-DA 0.032 0.113 0.10 0.81 0.019 0.059 0.92 0.087 0.051 0.172 1.02 0.91
 

FSV-DB
 0.052 0.160 0.64 0.70
 

FSV-DJ
 

FSV-DL
 0.066 0.161 0.64 0.58
 

FSV-DP
 

FSV-DQ
 0.052 0.138 0.58 0.81
 

FSV-DR
 

FSV-DS
 

FSV-DU
 

FSV-EI 0.044 0.129 0.14 0.79 0.043 0.079 0.85 0.135 0.087 0.208 0.99 0.92 

FSV-EL
 

FSV-EM
 1.890 1.160 1.620 1.650 

FSV-FN 

n 13 13 12 12 10 11 10 10 25 25 25 25 2 2 2 2 

Min 0.018 0.098 0.09 0.25 0.009 0.023 0.04 0.059 0.027 0.102 0.53 0.58 1.846 1.130 1.620 1.650 

Median 0.037 0.119 0.16 0.76 0.013 0.037 0.73 0.090 0.052 0.160 0.84 0.82 1.868 1.145 1.772 1.808 

Max 0.050 0.210 1.02 0.91 0.043 0.089 0.95 0.136 0.087 0.250 1.34 1.27 1.890 1.160 1.923 1.967 

eSD 0.010 0.021 0.09 0.09 0.006 0.013 0.24 0.020 0.013 0.040 0.27 0.18 

eCV 28 17 55 12 42 36 33 22 26 25 33 22 

NISTa
 

NISTb
 

NAV 

NAU 

0.045 0.118 0.13 0.68 0.023 0.027 0.75 0.078 0.068 0.146 0.88 0.75 

0.041 0.119 0.14 0.72 

0.011 0.027 0.19 0.19 

0.018 0.032 0.74 0.084 

0.010 0.017 0.27 0.028 

0.060 

0.016 

0.153 

0.043 

0.86 

0.25 

0.79 

0.19 

All Lab Report C5 Page 4 / 6 
Round Robin XXXIX Laboratory 

Analytes Reported By One Laboratory 

Values in μg/mL 

Term 

n 

Min 

Median
 

Max
 

eSD 

eCV 

NAV 

NAU 

nd 

nq 

>x 

! 

italics

Analyte Code 227 228 229 230 

cis-Lutein&Zeaxanthin FSV-BT 0.061 0.100 0.112 0.119 

Coenzyme Q10 FSV-CH 0.249 0.227 0.288 0.269 

trans-α-Carotene NISTb 0.034 0.024 0.017 0.104 

Legend 

Definition

 Number of (non-NIST) quantitative values reported for this analyte

 Minimum (non-NIST) quantitative value reported
 

 Median (non-NIST) quantitative value reported

 Maximum (non-NIST) quantitative value reported

 Estimated standard deviation, calculated from the median absolute deviation

 from the median of the non-NIST results

 Coefficient of Variation for (non-NIST) results: 100*eSD/Median

 NIST Assigned Value, our estimate of the "true" analyte concentration
 

 NIST Assigned Uncertainty, our estimate of the total (serum hetergeniety and

 inter- and intra-laboratory) standard deviation

 For details on how we assign these quantities, see the "Analysis of Results."

 Not detected (i.e., no detectable peak for analyte)

 Detected but not quantitatively determined

 Concentration greater than or equal to x

 Discrepant value: heterogeneous serum, damaged sample, malfunction, etc.

 Not explicitly reported but calculated by NIST from reported values

All Lab Report C6 Page 5 / 6 
 

 

 

 

Lab 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BGa 

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-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 

FSV-CH 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CP 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CT 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DJ 

FSV-DL 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DS 

FSV-DU 

FSV-EI 

FSV-EL 

FSV-EM 

FSV-FN 

NISTa 

NISTb 

n 

StS 

1
 

2
 

3
 

4
 

Round Robin XXXIX Laboratory Results
 

Comparability Summary
 

Definition
 

1 1 1 1 1
 

R aT gT bC tbC Label 

Lab laboratory number
 

1 1 1 1
 R "Standard Score" for Retinol
 

4 2 1 1
 aT "Standard Score" for α-Tocopherol 

2 2 2 1
 gT "Standard Score" for γ-Tocopherol 

2 3
 bC "Standard Score" for Total β-Carotene 

1 1 3
 tbC "Standard Score" for trans-β-Carotene

n number of (non-NIST) laboratories providing data for this analyte
 

3 1 4
 

2 2 1 1
 

1 1 2 2 2
 

2 1 1 1 1
 

2 1 1 2
 

2 1 1 2
 

"Standard Score" 

2 1 2 4
 Given that our knowledge of the shape, location, and width of the measurement
 

2 4 2
 distributions is approximate and that a limited number of labs are involved, we summarize
 

2
 comparability with the following four-level "Standard Score" (StS)...
 

1 4
 

1 1 1 1
 StS Definition

1 2 1 All StV within ±t (1-0.683,n-1) {i.e., ±1 SD}
 

1 1 2 All StV within ±t (1-0.954,n-1) {i.e., ±2 SD}
 

1 2 1 3 All StV within ±t (1-0.997,n-1) {i.e., ±3 SD}
 

1 1 1 2 4 At least one StV > ±t (1-0.997,n-1) {i.e., >3 SD}
 

1 1 1 1
 

4 1 2 3
 where:
 

1 2 1 3
 StV Standardized Value, the distance in standard deviation units your

3 1
 value is from the "true" concentration: StV = (your value - NAV) / NAU
 

1 2 3
 

1 1 2 1 1
 NAV NIST Assigned Value, our estimate of the "true" analyte concentration

3 2 1 1
 

2 1 2
 NAU NIST Assigned Uncertainty, our estimate of the total measurement

2 2 3
 standard deviation (serum heterogeniety, analytical repeatibility,

2 2 3
 and among-laboratory reproducibility)

2 2 4
 

2 2 2 1 1
 t (1-α,n-1) Two-tailed Student's t for coverage of ±1, ±2, and ±3 NAU about

2
 NAV, assuming a normal population of size n
 

2 1
 

4 4
 

4 4 2 2
 

4 1
 

1 2 4
 

2 2 2 3
 

3 2 2
 

3 3 2 1
 

1 1 2 1 1
 

1
 

2
 

1 2 2 2
 

1 1 2 4
 

1 2
 

2 1 1 2
 

1 1
 

1 1 1
 

4 4 3
 

1 1 2
 

2 3 2 2
 

2 4
 

1 2 1
 

1 1 2
 

1 1 1 1 1
 

1 1 1 1 1
 

54 52 30 37 11
 

% Observed Expected
 

61 72 78 54 69
 68.2 % These are the observed and normal-population-expected proportions of
 

29 15 16 33 23
 27.3 % each Standard Score (StS), based upon each laboratory's largest StV for the 

5 11 0 8 0 4.3 % four sera.

5 2 6 5 8
 0.3 % 

All Lab Report C7 Page 6 / 6
 
 

 

 

 

 

Appendix D. Representative “Individualized Report” for RR39 

Each participant in RR39 received an “Individualized Report” reflecting their reported 

results. Each report included a detailed analysis of the results they reported for some or 

all of the following analytes: 

• Retinol 

• Retinol palmitate 

• α-Tocopherol 

• γ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total α-Carotene 

• Total Lycopene 

• β-Cryptoxanthin 

• Lutein 

• Lutein & Zeaxanthin 

The software used to generate the original RR39 “Individualized Reports” is no longer 

available and we do not have hardcopy of the report as it was sent to any participant or 

NIST analyst. The following 11 pages were produced for participant FSV-BA using a 

descendant of the 1997 software. Three of the graphical tools used in the original reports 

(“Boxplot Comparisons”, “Z-Score Concordance”, and “NIST Assigned Values Vs 

Laboratory Values”) have been retained and display the same information in much the 

same manner as in the original. However, the original report presented the same type of 

information for a number of analytes together on one or two pages rather than presenting 

all information for a given analyte on a single page. The modern software does not 

provide the “% RSD Bias and Precision History” table or the “% Difference” plots. 

D1
 
 

 Set 1 of 57 

Individualized Round Robin XXXIX Report: FSV-BA 

Summary 

Serum 227 Serum 228 Serum 229 Serum 230 

Analyte You NAV n You NAV n You NAV n You NAV n 

Retinol 0.853 0.872 53 0.502 0.490 54 0.406 0.377 53 0.707 0.666 53 

Retinyl Palmitate 0.243 0.241 14 0.104 0.086 14 0.095 0.108 14 0.161 0.190 14 

α-Tocopherol 17.38 17.35 51 7.9 7.7 52 7.3 7.0 51 11.37 10.87 51 

γ-Tocopherol 3.86 3.67 30 1.92 1.70 30 4.44 4.26 30 1.51 1.29 30 

Total β-Carotene 1.224 1.235 37 0.181 0.169 37 0.119 0.104 36 0.131 0.100 37 

trans-β-Carotene 1.166 1.135 11 0.172 0.153 11 0.112 0.095 11 0.123 0.093 11 

Total cis-β-Carotene 0.058 0.103 8 0.009 0.012 7 0.007 0.010 6 0.008 0.008 6 

Total α-Carotene 0.056 0.049 30 0.035 0.025 30 0.028 0.017 30 0.155 0.119 31 

trans-Lycopene 0.181 0.165 8 0.266 0.220 8 0.478 0.421 8 0.296 0.236 8 

β-Cryptoxanthin 0.049 0.034 27 0.073 0.047 27 0.046 0.048 27 0.087 0.066 27 

Lutein&Zeaxanthin 0.061 0.060 25 0.208 0.153 25 1.330 0.855 25 1.270 0.786 25 

You : Your reported values for the listed analytes (micrograms/milliliter) 

NAV : NIST Assigned Values, here equal to this RR's median 

n : Number of non-NIST laboratories reporting quantitative values for this analyte in this serum 

Please check our records against your records. Send corrections and/or updates to... 

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology Tel: (301) 975-3935 

100 Bureau Drive Stop 8392 Fax: (301) 977-0685 

Gaithersburg, MD 20899-8392 USA Email: david.duewer@nist.gov 

Individualized Report Page 1 / 10 D2
 

 

 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

Retinol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein. 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 2 / 10 

D3
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

Retinyl Palmitate, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 3 / 10 

D4
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

α-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 4 / 10 

D5
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

γ-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 5 / 10 

D6
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

Total β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

D5

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 6 / 10 

D7
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

trans-β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 7 / 10 

D8
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

Total α-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 8 / 10 

D9
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

Total β-Cryptoxanthin, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 9 / 10 

D10
 
 

 

 

 Set 1 of 57 

Individualized RR XXXIX Report: FSV-BA 

Total Lutein&Zeaxanthin, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

202210227223225228229230 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#227 Lyophilized, multi-donor, native. This is the High level of SRM 968b. RR32 #202, RR34 #210 

#228 Lyophilized, single donor, augmented with retinyl palmitate. RR38 #223 and #225 

Lyophilized, prepared a "low normal" serum pool, augmented with: #229 New retinyl palmitate, γ- and δ-tocopherol, lycopene, and lutein.
 

Lyophilized, prepared a "low normal" serum pool, augmented with: retinol,
 

#230 retinyl palmitate, α- and γ-tocopherol, α-carotene, β-cryptoxanthin, lycopene, New
 

and zeaxanthin.
 

Individualized Report Page 10 / 10 

D11
 
 

 

Appendix E. Shipping Package Inserts for RR40 

The following two items were included in each package shipped to an RR40 participant: 

• Cover letter 

• Datasheet 

The cover letter and datasheet were enclosed in a sealed waterproof bag along with the 

samples themselves. 

E1
April 7, 1997 

Dear Colleague: 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg. Maryland 20899-

Enclosed is the set of samples for the second quality assurance round robin exercise (Round Robin XXXX) 

for FY97. You will find one vial of each of four lyophilized serum samples 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. If an obtained value is below your limit of quantitation, please indicate this result 

on the form by using NQ (Not Quantitated). For analytes not measured, please leave a blank. Results are 

due to NIST by June 13, 1997. Results received two weeks after the due date will not be included in the 

summary report for this round robin study. Written feedback concerning the study will be provided 

around July 25, 1997. 

Samples should be reconstituted with 1.0 mL ofHPLC-grade water or equivalent. We recommend that 

dissolution be facilitated with 3 to 5 min 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 that 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 LC systems creating analytical problems.) Pipette a known 

volume of serum from the vial for analysis. (The final volume of the reconstituted sample is greater than 

1.0 mL.) For consistency, we request that laboratories use the following absorptivities (E 1 % cm) in 

ethanol: retinol, 1850 at 325 nm; retinyl palmitate, 975 at 325 nm; a-tocopherol, 75.8 at 292 nm; 

y-tocopherol, 91.4 at 298 nm; a-carotene, 2800 at 444 nm (in hexane); ~-carotene, 2560 at 450 nm (in 

ethanol), 2592 at 452 nm (in hexane); lycopene, 3450 at 472 nm (in hexane). 

Please mail or fax your results for Round Robin XXXX to: 

Micronutrients Measurement Quality Assurance Program 

NIST 

Bldg. 222, Rm. B208 

Gaithersburg, MD 20899 

Fax: (301) 977-0685 

If you have questions regarding this round robin exercise, please call me at (301) 975-3120; 

ail me atjeanice.bro-w om @nist.gov; or mail/fax queries to the above address. 

J nice Brown Thomas 

esearch Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

cc: S. Wise 

E2
 

 

 

 

NIST/NCI
 

Micronutrients Measurement Quality Assurance Program
 

Round Robin XL Results from Laboratory #_____ 

Serum 

Analyte 231 232 233 234 Units* 

retinol 

retinyl palmitate 

α-tocopherol 

γ-tocopherol 

δ-tocopherol 

total β-carotene 

trans-β-carotene 

total cis-β-carotene 

total α-carotene 

trans-α-carotene 

total lycopene 

trans-lycopene 

β-cryptoxanthin 

lutein 

zeaxanthin 

lutein&zeaxanthin 

Other Analytes?
 

* We prefer mg/mL 

Today's Date: 

Comments? 

Mail: MMQAP, 222/B208 

NIST Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899 June 15, 1997 Email: David.Duewer@NIST.gov 

E3
Appendix F. Final Report for RR40

The following 11 pages are the final report as provided to all participants: 

•	 Cover letter and brief description of study design and overall results 

•	 A “Report of Analysis” that: 

o	 describes the nature of the test samples and details any previous distributions 

o	 summarizes aspects of the study that we believe may be of interest to the 

participants 

o	 details the analysis of the NIST results 

F1
 
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August 14, 1997 

Dear Colleague: 

-- -~----------

UNITED STATES DEPARTMENT OF COMMERC 

National Institute of Standards and Technolog 

Gaithersburg, Maryland 20899-0001 

Enclosed is the summary report of the results for Round Robin XL (RR40). Included in this 

report are: a summary of data for all laboratories; the measurement comparability summary for 

evaluating laboratory performance; a summary of individual laboratory performance for the past 

three years; a summary of the interlaboratory accuracy and precision over the same period of 

time for the measurement ofretinol, ix- and y-tocopherol, and trans- and total ~-carotene; and a 

graphical summary of the NIST assigned value (NA V) vs. your laboratory value for these 

analytes. As in previous reports, the NIST assigned values are derived from the equally 

weighted results from the analyses performed by NIST and the laboratories that participated in 

this interlaboratory comparison exercise. 

The experimental design for this interlaboratory comparison exercise is summarized below. The 

four serum samples (Sera 231-234) distributed in RR40 address the following issues: 

• Serum and Measurement Stability. Serum 234 is the mid level component of SRM® 968b. It 

was previously distributed as sera 201 and 209. Reanalysis of such well-characterized materials 

documents both the continued stability of the material and the "absolute accuracy" of the analyte 

level assignments. No significant changes in analyte concentrations were observed. 

• Analyte Augmentation Techniques. Sera 231, 232, and 233 were prepared from the same 

serum pool as models for the proposed Serum 968c. We again had mixed success, achieving 

nearly our target levels with many of the minor analytes, but completely missing the mark with 

et-tocopherol. We will re-evaluate our augmentation techniques and continue to explore ways to 

achieve sufficient levels of the analytes of interest. We apologize for any inconvenience caused 

by our aggressive (and sometimes unsuccessful) augmentation experiments. 

•Measurement Precision and Concordance. For several years now, we have been working 

toward a different evaluation/presentation of measurement quality. We now introduce the "ZScore Concordance" plots. These are experimental and may be significantly changed/deleted, 

but they were received with some interest at the QA Workshop in Atlanta 

The concepts necessary for "properly" evaluating measurement quality are debatable. While we 

are still struggling with both concepts and words, here is a synopsis. The common basic concept 

is "accuracy" - usually interpreted as "closeness to truth" (or at least to a knowable "limiting 

mean"). Through repeated measurements over time on the same material(s), two different 

aspects of measurement accuracy can be identified: "bias" and "precision." "Bias" can be 

interpreted as the average difference from "truth; "precision" can be interpreted as the amount of 

scatter in the individual differences. We've used these words in the "Individualized Report," 

estimating "accuracy" as the average 

% Bias= lOO*(NAV - your value) I NAV 

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taken over all the sera in the Round Robin and estimating "precision" as the standard deviation of 

the % bias values. 

The primary goal of the program is to get all participants to measure usefully similar values for 

different types of serum samples. Thus, for our purposes, concordance is how well the 

laboratories agree among themselves. As with accuracy, concordance also has two components. 

Rather than invent new words, we use "Average Concordance" for the "on average, how close?" 

component and "Concordance Consistency" for the "how much scatter?" component. 

The estimated expected uncertainties are used to assign the NIST Assigned Uncertainty or 

"NAU" values; the NAU values are used in calculating the "Comparability Summary" scores. 

The "comparability" scores are based on your standardized values (StV): 

StV = (Your value - NA V)/NAU 

This is a specific case of "Z-score" standardization. We have chosen to define the "Z-Score 

Concordance" values as: 

ZSC = (Your Value - Median)/NAU 

to remove any "NIST bias." The "Average Concordance" is the average of the ZSC values over 

all the sera analyzed, and the "Concordance Consistency" is the standard deviation of the ZSC 

values. As a minor complication, we average across related analytes (total and trans ~-carotene 

and lycopene) to allow more information to be compressed onto a single page. 

3 j Retinoi 

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-2 

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e You 

---TC=I 

------TC=2 

-1 0 1 2 3 

Average Concordance .,. 

Each of the analyte (or analyte group) plots shows the total "Z-Score Concordance" values for all 

participants in RR40. Your values are shown as a black square. and the two NIST analysts' 

values are shown as open circles. Ideally, everyone should duster very close to the "O" value: 

Average Concordance of zero, Concordance Consistency of zero. As a rough guide, we believe 

that the "good" values fall inside the inner semicircle. 

TC= Total Concordance= ~(AverageConcordance)2 + (ConcordanceConsistency)2 = l 

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However, while there is a tendency for consistency to decrease as the average moves away from 

zero, there are some laboratories that are very consistent yet rather far away from the median. 

Since this is clearly better than being high on one sample and low on another, we are still 

considering how best to "grade" the Total Concordance values. 

3 

Data for evaluating laboratory performance in RR40 are provided in the comparability summary 

(Score Card) on page 6 of the "All Lab Report." The criteria used to evaluate laboratory 

performance are as follows: results rated 1 (within 1 SD of the assigned value) indicate 

EXCEPTIONAL performance, results rated 2 (within 2 SD) indicate ACCEPTABLE 

performance, results rated 3 (within 3 SD of the assigned value) are MARGINAL, and those 

rated 4 (> 3 SD from the assigned value) indicate POOR performance relative to the current stateof-the-practice for these measurements. 

If you have concerns regarding your laboratory performance or were rated "POOR" based on the 

criteria stated above, we suggest that you obtain a unit of SRM 968b, Fat-Soluble Vitamins and. 

Cholesterol in Human Serum, and analyze all three levels. If, with minor modifications, your 

measured values do not agree with the certified values, we suggest that you contact us for 

consultation. 

The Micronutrients Measurement QA Workshop was held prior to the American Association 

Clinical Chemistry (AACC) meeting on July 20 at the Best Western American Hotel in Atlanta, 

Georgia. At the workshop there was some discussion regarding fundamental changes for future 

presentation of results and the identification of sources of bias among the laboratories. 

Regarding the latter, program participants will be asked to provide updated information on 

methodology, techniques, and other chromatographic parameters more routinely to help refine 

our database. Participants also expressed their interests in having materials characterized for 

folates, phytoestrogens, homocysteine, polyamines, and curcumin. Primary standards for 

compounds typically measured in the program (such as lycopene) were also on the "wish" list. 

Based on the workshop attendance, it appears that most of the veteran QA participants generally 

do not attend the AACC meeting. Since there was greater attendance when the workshop was 

held with the Experimental Biology meeting in 1996, it was suggested that our next workshop be 

held in conjunction with the 1999 Experimental Biology meeting in Washington, DC. We will 

keep you informed of the workshop plans as they are finalized. 

We also plan to hold the Fat-Soluble Vitamin and Carotenoid Analysis Tutorial again this 

fall at NIST, provided there is adequate interest. The scheduled date for the session is October 

27, 1997. This tutorial is intended primarily for new laboratories, new laboratory personnel, or 

those currently experiencing difficulties with their analysis. As in past years, this session will 

include a discussion of calibration, sample preparation, and chromatographic techniques for 

measuring fat-soluble vitamins and carotenoids in serum. 

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Enclosed are copies of the following publications: 

• Liquid Chromatographic Measurement of L-Ascorbic Acid and D-Ascorbic Acid in 

Biological Samples, Margolis, S.A. and Schapira, R.M., J. Chromatogr. B, 690 (1997) 25-33. 

• Certification of Nutrients in Standard Reference Material 1846: Infant Formula, 

Sharpless, K. E., Schiller, S.B., Margolis, S.A., Brown Thomas, J., Iyengar, G.V., Gills, T.E., 

Wise, S.A., Tanner, J.T., and Wolf, W.R., J. AOAC, 80 (1997) 611-21. 

Other recent publications of note are: 

• Reference values for retinol, tocopherol, and main carotenoids in serum of control and 

insulin-dependent diabetic Spanish subjects. Olmedilla B., Granado F., Gil-Martinez E., 

Blanco I., and Rojas-Hidalgo E. Clin. Chem. 1997:43(6);1066-1071. Prof. Olmedilla can be 

contacted at: bolmed@nutr.cph.es or Servicio de Nutricion, Clinica Puerta de Hierro, 28035 

Madrid, Spain. 

4 

• NHANES III, Reference Manuals and Reports CD-ROM (October 1996), National Center 

for Health Statistics, Centers for Disease Control and Prevention, Hyattsville, MD 20782, Phone: 

(301) 436-8500, FAX: (301) 436-4258; e-mail: SETS@nchlOa.em.cdc.gov. 

Samples for RR41 were shipped during the last week of July. Results are due September 19; 

feedback to labs will be provided around October 27. 

If you have any questions regarding this report, please contact me at 3011975-3120; FAX: 

301/977-0685; e-mail: jeanice.brownthomas@nist.gov. 

Sincerely, . /1,w/ if)'l(fl/J 

Jl::wn Thomas 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

cc: S. Wise 

Enclosures 

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The attached N2M2QAP Round Robin XL (RR40) Feedback includes the standard "All Lab" 

report: 

Page 

1-4 

Sa 

Sb 

6 

"All Lab" Report Contents 

A listing of all results for analytes reported by at least two laboratories, plus 

essential summary statistics 

A list of results for the analytes reported by only one laboratory 

A legend for the above two lists 

The "Measurement Comparability Summary" (or "Score Card") 

The order of many components of the "Individualized" report has been changed to allow easy 

deletion of "empty" %bias plots. Also, we've added an experimental set of "concordance" charts 

to help you evaluate the performance characteristics of your measurements. 

Page 

1 

2, 3 

4 

s 

6 

7-9 

"Individualized" Report Contents 

Your values, our assigned values, and the %bias between the two 

"Comparisons" plots for: retinol, retinyl palmitate, tt- and y-tocopherol, total 

and trans-p-carotene, total et-carotene, total lycopene, p-cryptoxanthin, lutein, 

and lutein&zeaxanthin 

"Z-Score Concordance" plots for this RR's: retinol, tt-tocopherol, ytocopherol, total and trans-p-carotene, total et-carotene, and total and translycopene. 

% Bias Accuracy/Precision Summary for your last 3 years' results 

Our assigned value vs. your value scatterplots for retinol, tt- and ytocopherol, and total and trans-p-carotene, also for your last 3 years' results 

% Bias barchart for retinol, tt- and y-tocopherol, and/or total and trans-Pcarotene for your last 3 years' results. Only plots showing some data are 

included! 

F6
 
Analysis of Results Round Robin XL: Sera 231-234 

Analysis of N2M2QAP Round Robin XL Results: Sera 227 to 230 

Background: The following four samples were distributed in RR40 

Sera 231-233: experimental sera, prepared from a single "low" serum pool and augmented 

with the various analytes to (try to) hit 10%, 50%, and 90% population levels. We did with 

some, not with others. We also over-spiked retinyl palmitate, to try to get a level that 

everyone could measure well. 

Page 1 

Serum 234: the "middle level" component of SRM® 968b: Fat-Soluble Vitamins and 

Cholesterol in Human Serum. It was previously distributed as serum 201 in RR32 (9/94) and 

serum 209 in RR34 (6/95). 

Qualitative Results: The following observations were noted in the RR40 reports: 

Several participants obtained consistently low retinol values for the experimental sera, 231-

233, while getting the mid-level 968b serum dead on. This suggests a systematic methodrelated bias. One of the workshop attendee's suggested that this may reflect differences in 

protein denaturation. 

Action: This is a very important observation! We will re-examine old data, now that we 

know what to look for. But, to figure out the mechanism, we need your help! If 

you all are willing, we'd like to collect details on your total analytical method. 

We'll try to figure out the least painful way to do this, both for you and for us, and 

get started on this in early Fall. 

One participant noted that the amber vials are too small. 

Action: Sigh. We've only been able to locate these 2.0 and 5.0 mL ambers, and the 5.0's 

are just to big for our production methods. Sorry. If someone can locate 2.5 to 

3.0 mL ambers for a reasonable price, we'll consider changing ... 

One participant noted with enthusiasm our success at achieving a high J3-cryptoxanthin levels. 

Action: We're trying, we're trying ... 

Quantitative Results The following NIST Data and Value/Uncertainty Assignments table 

presents all NIST data, summary statistics for the NIST data, summary results for RR40, and 

the NIST assigned values and uncertainties. The entries are defined as follows: 

Individual NIST Analyst Data and Summazy Statistics 

A: 1 to C:2 two aliquots ("1" and "2") of three vials (A, B, and C) of each serum were 

extracted and analyzed. Each analyst analyzed a separate set of three vials. 

llx number of quantitative values for this analyte for this serum for this analyst 

Me~ arithmetic average 

SDx simple standard deviation 

SDrqix within-vial pooled standard deviation, reflecting variation in extraction, 

chromatography, peak integration, etc. 

SD11eix among-sample standard deviation, reflecting heterogeneity in preparing and 

reconstituting the serum samples 

_________ 

231 to 234
­

F7
 
Analysis of Results Round Robin XL: Sen 231-234 

SDNlSTx ~SD~x +SD~ , total standard deviation. This value is ~ SDx, as sample 

replicates reduce the true degrees of freedom. 

CV N1STx 100 x SD NISTJMean1 

NIST Summazy Statistics 

n number of quantitative values for this analyte for this serum 

Mean (MeanNIST1 + MeanNJS13)/2 or MeanNlST3 for analytes that NISTl did not report 

SDrep within-vial pooled standard deviation 

SDbet among-sample standard deviation 

Pagel 

soul between-analyst standard deviation. This is the residual standard deviation for 

regression of NIST3' s Me~ values to NIST l's or, for analytes that NISTl did 

not report, to the interlaboratory Median (see below). The model used to 

determine SDan1 is defined to the right of this block. Details include: model used, 

parameters and standard errors on the parameters, and R2 • 

SDNIST ~SD~ +SD~, + SD!i1 , total standard deviation for NIST analyses. 

CV NIST 100 x SDNIStMean 

Round Robin XL Summary Statistics 

n. number of non-NIST laboratories reporting quantitative values for this analyte 

for this serum in this Round Robin 

Mediann median of the reported values 

eSDD 0.741 x InterQuartile Range (IQR) 

P(n=p) TDIST( IMediann -MedianPl~-nn_+_n_P ___ 2 , ~+nn-2, 2-tail) 

(<nD - l)eSD! + (np -l)eSD!)(-

1 

+-

1 

) 

nn nP 

This is the approximate probability that the current median is the same as it was 

in its initial distribution. Where the hypothesis that Mediann = Medi~ can be 

rejected with 95% confidence, the P(n=p) value is flagged with an"*". TDIST 

is Excel~'s student's t function. 

. SD2 

P(n<p) FOIST( 4, nD-1, ~-1) eSD0 

This represents the approximate probability that the current interlaboratory 

variance is smaller than it was in its initial distribution. Where the hypothesis 

that eSD11 < eSDR can be rejected with 95% confidence, the P(n<p) value is 

flagged with an *". FOIST is Excel~' s F-distribution function. 

SDllhl ~eSD!-SD~, the residual non-NIST interlaboratory biases after correction 

for measurement-, sampl~. and NIST-analyst-related sources of variance. When 

SDNJST is greater than eSDn, SDllhl = 0. 

CV llhl l 00 x SD...JMedi&I\ 

F8
 
Analysis of Results Rowid Robin XL: Sera231-234 Pap3 

N.IS_T Assigned Values and Uncertainties 

NA V (Mean + Mediann) I 2, our best guess of the "true" analyte level 

NAU Maximum( 0.05 x NA V, ~SD~T +SD~ ), our best guess for the "true" 

interlaboratory standard deviation characterizing measurement, sample 

heterogeneity' interanalyst, and interlaboratory sources of variation. When SD labs 

could not be determined, NAU is estimated as 

Maximum(0.10 x NAV, ~2 SD~T ). 

CV lOOxNAU/NAV 

Measurement Performance Summary: The following is based on results presented in the 

NIST Data and Value/Uncertainty Assignments table of this report and the "Individualized 

Report" page 2 and 3 summary graphs: 

Serum 234. mid-level SRM 968b. stability: There is no significant difference in the level or 

measurement variability of any analyte among the three analyses of this material (sera 201, 

209, and 234). 

Action: Thankfully, none required. 

Sera 231- 233 homogeneity: It is probable that these materials are less homogenous than 

desired, particularly for a-tocopherol where considerably less was observed than was spiked! 

Action: This is an ongoing problem and major concern. We are considering revising the 

various "grade sheets" for this RR40, perhaps just to reflect the SRM 968b values. 

More on this in the RR41 package! Only enough of these sera were produced for 

this one RR, so you WQn 't see them again. 

Retjnyl palmitate: The CVs for all sera are 20-30%, nearly independent of analyte level. 

Action: RP remains analytically challenging! The community needs to develop better 

techniques if this analyte is of importance. For now, don't believe any RP 

numbers! 

~~ 

DaveDuewer ~ 

Research Chemist 

David.Duewer@NIST.gov 

/~~ Research Biologist 

Margaret.Kline® NIST.gov 

F9
 
Analysis Results Round Robin XL: Sera 231- 234 

NIST Data and Value/Uncertainty Assignments 

Retinol 

NISTl NIST3 

231 232 233 234 231 232 233 234 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

0.251 0.349 0.807 0.467 0.250 0.421 0.783 0.506 

0.275 

0.261 

0.250 

0.243 

0.224 

n, 6 

Mean I 0.251 

SD 

so .... SDi.u 

I 0.017 

I 0.013 

O.ot5 

0.333 0.786 

0.351 0.748 

0.495 0.738 

0.401 0.808 

0.489 0.794 

6 6 

0.403 0.780 

0.073 0.030 

0.069 0.011 

0.055 0.032 

0.481 0.263 0.443 0.812 

0.488 0.263 0.425 0.789 0.504 

0.517 0.256 0.419 0.784 0.495 

0.415 0.264 0.417 0.775 0.499 

0.483 0.258 0.403 0.734 0.496 

6 6 6 6 5 

0.485 0.259 0.421 0.779 0.500 

0.017 0.005 0.013 ·0.025 0.005 

0.013 0.006 0.011 0.021 0.004 

0,015 0.002 0.011 0.022 0.004 

SDNIS'TI 0.021 0.088 0.034 0.020 0.007 0.015 0.030 0.006 

CVNlm 8.2 22 4.4 4.2 2.7 3.6 3.9 1.2 

n 

Mean 

so_ 

so.. 

so ... Sl>wm 

CVNIST 

RR 

Scrum 

n., 

Median0 

cSD11 

n. 

Median, 

cSD1 

P(n:o:p) 

P(n<p) 

12 

0.255 

0.011 

0.010 

0.010 

0.018 

7.0 

231 

42 

0.265 

0.034 

SDw. 0.029 

cv..,.. 11 

NIST 

12 12 11 

0.412 0.780 0.493 

0.049 0.012 0.010 

0.035 0.024 0.011 

0.010 0.010 0.010 

0.061 0.029 0.018 

15 3.7 3.6 

XXXIV 

209 

48 

0.530 

0.050 

RRXL 

232 233 2.34 

43 43 43 

0.421 0.770 0.509 

0.048 0.058 0.033 

0.92 

1.00 

0 0.050 0.028 

0 6.5 5.6 

NAV 0.260 0.417 0.775 0.501 

NAU __...06_1..__. .0 .-.. 3 

CV 13 IS 1.S 6.1 

xCV 10 9.0 8.8 8.8 

NIST3=a+b*NIST I 

a: 0.020 :t0.014 

b: 0.977 ±0.026 

R2

: 0.999 

<-Current Results- > 

<- Assignments- -> 

Retinyl Palmitate 

NISTl NIST3 

231 232 233 234 

0 0 0 0 

NIST 

5 6 6 6 

1.02 1.40 0.182 0.151 

0.10 0.04 0.027 0.016 

0.15 0.10 0.030 0.009 

0.03 0.03 0.034 0.034 

0.18 0.11 0.053 0.039 

18 8.1 29 26 

X:X:XIV 

209 

13 

0.19 

0.02 

RRXL 

231 232 233 234 

14 14 14 14 

0.77 1.07 0.186 0.179 

O.lS 0.32 0.043 0.025 

0.79 

0.07 

0 0.30 

0 28 

0 

0 

0 

0 

0.89 

0.18 

20 

20 

1.24 0.184 0.165 

0.32 0.053 0.039 

26 29 23 

20 24 25 

231 232 233 234 

0.84 1.31 0.213 0.161 

0.88 1.28 0.151 0.155 

1.07 1.38 0.160 0.141 

1.24 1.45 0.143 0.169 

1.07 1.48 0.224 0.154 

1.50 0.199 0.128 

5 6 6 6 

1.02 1.40 0.182 0.151 

0.16 0.09 0.034 O.ot5 

0.07 0.03 0.028 0.016 

0.15 0.10 0.030 0.009 

0.16 0.10 0.041 O.ot8 

16 7.4 22 12 

NIST3=a+b*Median 

a: -0.065 ±0.041 

b: 1.379 ±0.053 

R2

: 0.997 

F10
 
Analysis Results Round Robin XL: Seta 231-234 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean. 

so. 

so_ 

so._ 

231 

4.55 

5.43 

5.00 

4.62 

4.56 

4.16 

6 

4.72 

0.44 

0.42 

0.32 

a-Tocopherol 

NISTl 

232 233 234 231 

5.73 8.53 9.41 4.46 

5.87 7.94 9.32 4.31 

5.91 8.05 9.48 4.94 

8.14 7.88 9.95 4.93 

6.78 7.48 9.45 4.89 

7.47 8.08 9.44 4.94 

6 6 6 6 

6.65 8.00 9.51 4.74 

0.99 0.34 0.22 0.28 

0.95 0.35 0.20 0.06 

0.74 0.23 0.18 0.31 

NIST3 

232 233 234 

6.51 7.39 9.35 

6.02 7.46 

7.05 8.20 10.21 

7.01 7.91 10.05 

6.68 7.94 9.80 

6.68 7.30 9.78 

6 6 5 

6.66 7.70 9.84 

0.38 0.36 0.32 

0.20 0.29 0.06 

0.38 0.32 0.39 

SONISTa 0.53 1.20 0.42 0.27 0.32 0.43 0.43 0.39 

cvNIST. 11 18 5.3 2.8 6.7 6.5 5.6 4.o 

n 

Mean 

so. 

so... 

so .. SI>msr 

CVNIST 

RR 

Serum 

n. 

Median, 

eSO, 

n. 

Median. 

eSD, 

P(n=p) 

P(n<p) 

12 

4.73 

0.30 

0.27 

0.14 

0.43 

9.1 

231 

39 

4.87 

0.68 

SD11111 0.53 

CV11111 11 

NAV 4.80 

NAU 0.68 

CV 14 

xCV 9.8 

NIST 

12 12 

6.65 7.85 

0.69 0.28 

0.49 0.24 

0.14 0.14 

0.86 0.39 

13 5.0 

RRXL 

232 233 

39 39 

6.80 7.89 

0.58 0.86 

11 

9.67 

0.15 

0.43 

0.14 

0.48 

4.9 

XXXIV 

209 

47 

9.87 

0.85 

234 

39 

9.68 

0.71 

0.96 

0.88 

NIST3=a+b*NIST1 

a: 0.50 ±0.39 

b: 0.91 ±0.06 

R1

: 0.991 

<-Current Results -> 

0 0.76 0.52 

0 9.7 5.4 

6.73 7.87 

0.86 0.86 

13 11 

8.1 7.6 

9.67 <-Assignments-> 

0.71 

7.3 

7.3 

231 

1.46 

1.46 

1.46 

1.39 

1.34 

1.45 

6 

1.43 

0.05 

o.os 

0.03 

0.06 

4.4 

12 

1.43 

0.04 

0.03 

0.03 

0.06 

4.1 

231 

23 

1.36 

0.15 

0.14 

10 

1.40 

0.15 

11 

10 

"t Tocopherol 

NISTl 

232 233 

2.33 0.722 

2.36 0.703 

2.41 0.700 

3.32 0.725 

2.83 0.747 

3.01 0.772 

6 6 

2.71 0.729 

0.41 0.026 

0.38 0.015 

0.32 0.026 

0.50 0.030 

18 4.1 

NIST 

12 12 

2.68 0.730 

0.27 0.018 

0.20 0.023 

0.03 0.029 

0.34 0.041 

13 5.7 

RRXL 

232 233 

23 23 

2.85 0.770 

0.31 0.105 

0 0.096 

0 12 

2.n 0.750 

0.34 0.105 

12 14 

7.9 15 

234 

2.08 

2.04 

2.17 

2.34 

2.15 

2.15 

6 

2.16 

0.10 

0.00 

0.10 

0.12 

5.7 

11 

2.22 

0.05 

0.11 

0.03 

0.12 

5.6 

XXXIV 

209 

23 

2.39 

0.24 

234 

23 

2.29 

0.22 

0.90 

0.65 

0.19 

8.2 

2.25 

0.22 

9.9 

8.3 

NIST3 

231 232 233 234 

1.41 2.64 0.689 2.25 

1.39 2.57 0.725 

1.47 2.76 0.764 2.34 

1.46 2.75 0.740 2.31 

1.46 2.57 0.767 2.23 

1.45 2.58 0.703 2.26 

6 6 6 5 

1.44 2.65 0.731 2.28 

0.03 0.09 0.032 0.05 

0.01 0.03 0.031 0.02 

0.04 0.10 0.023 0.04 

0.04 0.10 0.039 o.os 

2.6 3.8 5.3 2.1 

NIST3=a+b*NIST1 

a: 0.044 ±0.038 

b: 0.963 ±0.021 

R1

: 0.999 

F11
 
Analysis Results Round Robin XL: Sera 231-234 6 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean. 

SD I 

SD..,... 

231 

1.10 

1.18 

1.15 

1.13 

1.15 

5 

1.14 

0.03 

0.03 

0.01 

&. Tocopherol 

NISTl NIST3 

232 233 234 231 232 233 234 

1.13 0.213 0.209 0.162 

1.12 0.196 0.235 

1.16 0.259 0.265 0.181 

1.15 0.242 0.238 0.182 

1.16 0.230 0.247 0.167 

1.16 0.237 0.242 0.170 

0 0 0 6 6 6 5 

1.15 0.229 0.239 0.172 

0.02 0.022 O.Q18 0.009 

0.00 0.010 0.015 0.001 

0.02 0.023 O.Q15 0.010 

Total p-Carotene 

NISTl NIST3 

231 232 233 234 231 232 233 234 

0.076 0.185 0.453 0.643 0.071 0.202 0.392 0.606 

0.076 0.269 0.446 0.589 0.067 0.211 0.405 

0.072 0.230 0.445 0.677 0.086 0.236 0.472 0.648 

0.069 0.224 0.460 0.657 0.083 0.255 0.463 0.652 

0.071 0.231 0.414 0.641 0.078 0.204 0.434 0.642 

0.079 0.243 0.466 0.642 0.075 0.235 0.441 0.642 

6 6 6 6 6 6 6 5 

0.074 0.230 0.447 0.642 0.077 0.224 0.434 0.638 

0.004 0.027 0.018 0.029 0.007 0.021 0.032 0.019 

0.004 0.035 0.022 0.024 0.003 0.015 0.007 0.001 

SDhco 0.003 0.006 0.007 0.025 0.008 0.020 0.035 0.024 

s~. o.o3 

CVNISTI 3.0 

0.02 0.025 0.022 0.010 0.005 0.035 0.023 0.035 0.008 0.025 0.035 0.024 

1.8 11 9.0 5.8 6.2 15 5.2 5.4 11 11 8.1 3.7 

NIST 

n 

Mean 

SD..., 

so... 

so. 

SI>wt 

CVNIST 

RR 

Serum 

n, 

Median, 

eSD, 

11 6 

1.15 0.229 

0.02 0.012 

0.02 0.023 

0.00 0.003 

0.03 0.026 

2.7 11 

6 5 

0.239 0.172 

0.019 0.000 

O.Q15 0.010 

0.003 0.003 

0.024 0.010 

10 6.0 

XXXIV 

~ 1 

RRXL 

n. 

Median. 

eSD, 

P(n=p) 

P{n<p) 

231 

4 

1.06 

0.12 

so .. 0.11 

cv...,. 11 

232 

3 

0.170 

0.006 

0 

0 

233 234 

3 3 

0.184 0.116 

0.011 0.031 

0 0.030 

0 26 

NIST3=a+b*Median 

a: 0.050 ±0.003 

b: 1.040 ±0.004 

R2

: 1.000 

<-Current Results-> 

NAV 1.10 0.200 0.212 0.144 <-Assignments-> 

NAU . 0.12 0.026 0.024 0.031 

CV 11 13 12 22 

xCV 

NIST 

12 12 12 11 

0.075 0.227 0.441 0.640 

0.003 0.026 0.016 0.017 

0.005 0.013 0.022 0.023 

0.002 0.002 0.002 0.002 

0.007 0.029 0.028 0.028 

8.7 13 6.3 4.4 

XXXIV 

209 

37 

0.617 

0.103 

RRXL 

231 232 233 234 

25 25 25 25 

0.074 0.219 0.494 0.610 

0.013 0.050 0.083 0.080 

0.98 

0.90 

o.oi 1 o.04o 0.018 o.075 

15 18 16 12 

0.075 0.223 0.467 0.625 

0.013 0.050 0.083 0.080 

17 22 18 13 

24 18 15 14 

NIST3=a+b*NIST1 

a: 0.005 ±0.003 

b: 0.959 ±0.009 

R2

: 1.000 

F12
 
Analysis Results Round Robin XL: Sera 231-234 7 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

231 

0.071 

0.074 

0.070 

0.065 

0.062 

0.076 

6 

• 0.070 

n, 

Mean 

SD 

SD'"" 

so._ 

• 0.005 

• 0.006 

0.003 

trans-~· Carotene 

NISTl NIST3 

232 233 234 231 232 233 234 

0.182 0.437 0.512 0.060 0.185 0.357 0.557 

0.258 0.377 0.539 0.056 0.182 0.367 

0.186 0.339 0.587 0.072 0.216 0.431 0.599 

0.212 0.371 0.524 0.073 0.230 0.428 0.589 

0.210 0.355 0.538 0.061 0.190 0.404 0.592 

0.187 0.358 0.553 0.069 0.212 0.404 0.593 

6 6 6 6 6 6 5 

0.206 0.373 0.542 0.065 0.202 0.399 0.586 

0.029 0.034 0.026 0.007 0.020 0.031 0.017 

0.034 0.028 0.028 0.004 0.011 0.004 0.004 

0.012 0.029 O.Ql5 0.007 0.020 0.034 0.021 

Total a-Carotene 

NISTl NIST3 

231 232 233 234 231 232 233 234 

0.052 0.024 0.107 0.043 0.045 0.018 0.129 0.039 

0.050 0.025 0.104 0.046 0.041 0.023 0.117 

0.052 0.025 0.097 0.034 0.057 0.020 0.123 0.045 

0.053 0.026 0.108 0.036 0.056 0.024 0.112 0.052 

0.050 0.027 0.104 0.035 0.059 0.020 0.107 0.042 

0.047 0.025 0.082 0.032 0.054 0.026 0.113 0.049 

6 6 6 6 6 6 6 5 

0.051 0.026 0.100 0.038 0.052 0.022 0.117 0.046 

0.002 0.001 0.010 0.005 0.007 0.003 0.008 0.005 

0.002 0.001 0.010 0.002 0.003 0.004 0.007 0.004 

0.002 0.001 0.007 0.006 0.008 0.001 0.007 0.005 

Sl>wisr. 0.007 0.036 0.041 0.032 0.008 0.022 0.034 0.022 0.003 0.001 0.012 0.006 0.008 0.004 0.010 0.006 

cvNIST. 9.8 18 11 5.9 13 11 8.6 3.7 5.3 5.2 12 16 15 18 8.3 14 

n 

Mean 

SDiee 

SD11o1 

so. 

Sl>msr 

CVNIST 

RR 

Serum 

n, 

Median, 

eSD, 

n, 

Median, 

eSD1 

P(n=p) 

P(n<p) 

so .. 

cv...,. 

NIST 

12 12 12 11 

0.067 0.204 0.386 0.564 

0.005 0.025 0.020 0.021 

0.006 0.016 0.030 0.017 

0.010 0.010 0.010 0.010 

0.013 0.031 0.037 0.029 

19 15 9.7 5.1 

XXXIV 

209 

11 

0.603 

0.046 

RRXL 

231 232 233 234 

10 10 10 10 

0.068 0.233 0.473 0.570 

0.009 0.059 0.062 0.049 

0.77 

0.42 

0 0.050 0.050 0.040 

0 22 10 7.1 

NIST3=a+b*NIST1 

a: -0.016 ±0.012 

b: 1.102 ±0.048 

R3

: 0.996 

<-Current Results-> 

NAV 0.068 0.218 0.429 0.567 <-Assignments-> 

NAU 0.013 0.059 0.062 0.049 

CV 18 27 14 8.7 

xCV 13 9.4 9.1 9.1 

NIST 

12 12 12 11 

0.051 0.024 0.108 0.042 

0.002 0.003 0.009 0.003 

0.005 0.001 0.007 0.007 

0.002 0.002 0.002 0.002 

0.006 0.003 0.011 

11 14 11 

RRXL 

231 232 233 

26 24 26 

0.047 0.015 0.107 

0.014 0.005 0.029 

0.013 0.004 0.027 

28 29 25 

0.008 

19 

XXXIV 

209 

23 

0.028 

0.011 

234 

26 

0.029 

0.008 

0.98 

0.94 

0 

0 

0.049 0.019 0.108 0.035 

0.014 0.005 0.029 0.008 

29 28 27 22 

28 32 26 29 

NIST3=a+b*NIST1 

a: -0.012 ±0.002 

b: 1.277 ±0.030 

R2:0.999 

F13
 
Analysis Results Round Robin XL: Sera 231-234 8 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

I 

I 

Mean, 

SD 

SD,.. 

SDi.u 

SDN1sr1 

CVNIST1 

n 

Mean 

so. 

so.. 

so .. S°"1sT 

CVNIST 

RR 

Serum 

n, 

Median, 

eSD, 

"· Median. 

eSD. 

P(n=p) 

P(n<p) 

SDw,. 

cv .... 

231 

0 

6 

0.05 

0.00 

O.ot 

231 

0 

trans-a-Carotene 

NISTl NIST3 

232 233 234 231 232 233 234 

0.04 O.ot5 0.12 0.02 

0.04 0.014 0.10 

0.05 0.016 0.11 0.03 

0.05 O.ot8 0.10 0.03 

0.04 0.017 0.10 0.03 

0.05 O.ot9 0.1 0 0.03 

0 0 0 6 6 6 5 

0.05 0.016 0.11 0.03 

0.01 0.002 0.01 0.00 

0.00 0.001 O.ot 0.00 

0.01 0.002 0.01 0.00 

0.01 0.002 O.ot 0.00 

14 15 8.8 16 

NIST 

6 6 5 

0.016 0.11 0.03 

0.001 0.01 0.00 

0.002 0.01 0.00 

XXXIV 

LJ 

RRXL 

232 233 234 <- CUrTCnt Results - > 

0 0 0 

:~~I 0.05 0.016 0.11 0.031 <- Assignments - > 

CV 

xCV 

Total Lycopene 

NISTl NIST3 

231 232 233 234 

0 0 0 0 

NIST 

6 6 6 5 

0.236 0.242 0.209 0.333 

0.005 0.015 0.009 0.004 

0.037 0.037 0.028 0.022 

0.019 0.019 0.019 0.019 

0.042 0.044 0.035 0.030 

18 18 17 8.9 

RRXL 

231 232 . 233 

26 26 26 

0.193 0.231 0.194 

0.050 0.060 0.049 

0.027 0.040 0.034 

14 17 18 

0.215 0.236 0.201 

0.050 0.060 0.049 

23 25 24 

26 26 26 

XXXIV 

209 

24 

0.276 

0.059 

234 

26 

0.272 

0.(177 

0.99 

0.10 

0.072 

26 

0.302 

0.077 

26 

25 

231 232 233 234 

0.198 0.218 0.176 0.311 

0.192 0.205 0.192 

0.260 0.270 0.244 0.357 

0.268 0.295 0.233 0.350 

0.257 0.225 0.186 0.313 

0.244 0.237 0.222 0.333 

6 6 6 5 

0.236 0.242 0.209 0.333 

0.033 0.034 0.028 0.021 

0.007 0.012 0.017 0.009 

0.037 0.037 0.028 0.022 

0.037 0.039 0.032 0.024 

16 16 15 7.1 

a: 0 

b: 1.107 :t<>.054 

R2:0.046 

F14
 
Analysis Results Round Robin XL: Sera 231-234 9 

NIST Data and Value/Uncertainty Assignments 

trans-Lycopene 

NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean. 

• SD 

so_ 

SDllcU 

SDNIS'flt 

CVmsn 

231 

0 

232 233 234 

0 0 0 

NIST 

n 6 6 6 5 

Mean 0.099 0.120 0.094 0.149 

SD,.. 0.002 0.007 0.004 0.002 

so... 0.012 o.ow 0.010 0.010 

so. 0.006 0.006 0.006 0.006 

SDNIS'f 0.014 0.022 0.012 0.012 

CVNIS'f 14 18 13 8.0 

RR 

Serum 

Dp 

Median0 

eSD0 

n. 

Median. 

eSD. 

P(n=p) 

P(n<p) 

231 

7 

0.108 

0.014 

RRXL 

232 233 

7 7 

0.128 0.112 

0.043 0.019 

XXXIV 

209 

6 

0.177 

0.047 

234 

7 

0.148 

0.038 

0.71 

0.69 

SD11119 0.002 0.037 O.ot5 0.036 

CVw. 2.2 29 13 25 

231 232 233 234 

0.087 0.105 0.081 0.136 

0.084 0.102 0.089 

0.108 0.136 0.103 0.158 

0.111 0.148 0.105 0.155 

0.100 0.112 0.092 0.148 

0.103 0.119 0.097 0.147 

6 6 6 5 

0.099 0.120 0.094 0.149 

0.011 0,018 0.009 0.009 

0.002 0.006 0.004 0.001 

0.012 0.020 0.010 0.010 

0.012 0.021 o.oi 1 0.010 

12 17 11 6.9 

NIST3=a+b*Median 

a:O 

b: 0.903 ±0.029 

R2

: 0.670 

<-Current Results -> 

NAV 0.103 0.124 0.103 0.148 <-Assignments-> 

NAU 0.014 0.043 0.019 0.038 

CV 13 34 18 26 

xCV 

p.Cryptoxanthin 

NISTl NIST3 

231 232 233 234 

0 0 0 0 

NIST 

6 6 6 5 

0.035 0.102 0.241 0.027 

0.001 0.005 0.007 0.002 

0.003 0.008 o.ois 0.003 

0.014 0.014 0.014 0.014 

0.014 0.017 0.022 0.014 

41 16 9.1 53 

RRXL 

231 232 233 

22 22 22 

0.047 0.138 0.270 

0.008 0.026 0.045 

0 0.019 0.039 

0 14 15 

XXXIV 

209 

17 

0.043 

0.013 

234 

22 

0.034 

0.013 

0.83 

0.57 

0 

0 

0.041 0.120 0.255 0.030 

0.014 0.026 0.045 0.014 

35 21 18 47 

29 23 20 31 

231 232 233 234 

0.032 0.096 0.225 0.023 

0.030 0.090 0.241 

0.037 0.105 0.261 0.027 

0.036 0.112 0.256 0.031 

0.039 0.102 0.239 0.025 

0.036 0.106 0.225 0.029 

6 6 6 5 

0.035 0.102 0.241 0.027 

0.003 0.008 0.015 0.003 

0.001 0.004 0.009 0.002 

0.003 0.008 O.ot5 0.003 

0.004 0.009 0.018 0.003 

11 8.9 7.4 13 

NIST3=a+b*Median 

a: -0.016 ±0.016 

b: 0.936 ±0.088 

R2

: 0.983 

F15
 
Analysis Results Round Robin XL: Seta 231-234 10 

NIST Data and Value/Uncertainty Assignments 

''Lutein" "Zeaxanthin" 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean. 

so. 

SD,_ 

so._ 

SOmST& 

CVNTSTa 

231 

0 

NISTl 

232 233 234 

0 0 0 

NIST3 

231 232 233 234 

0.143 0.240 0.052 0.067 

0.142 0.242 0.056 

0-.146 0.249 0.054 0.062 

0.143 0.244 0.053 0.066 

0.145 0.231 0.056 0.062 

0.146 0.236 0.058 0.066 

6 6 6 5 

0.144 0.240 0.055 0.065 

0.002 0.006 0.002 0.002 

0.001 0.003 0.002 0.002 

0.002 0.006 0.002 0.001 

0.002 0.007 0.003 0.002 

1.3 2.9 4.7 3.8 

NISTl NIST3 

231 232 233 234 231 232 233 234 

0.261 0.026 0.028 0.035 

0.258 0.027 0.030 

0.270 0.030 0.031 0.033 

0.263 0.030 0.029 0.036 

0.266 0.027 0.029 0.029 

0.266 0.028 0.029 0.033 

0 0 0 0 6 6 6 5 

0.264 0.028 0.029 0.033 

0.004 0.002 0.001 0.003 

0.003 0.001 0.001 0.002 

0.004 0.002 0.001 0.002 

0.005 0.002 0.002 0.003 

1.8 6.3 5.2 9.5 

NIST NIST3=a+b*Median NIST NIST3=a+b*Median 

n 6 6 6 5 

Mean 0.144 0.240 0.055 0.065 

SD,. 0.001 0.003 0.002 0.002 

so.. 0.002 0.006 0.002 0.001 

so.. 0.001 0.001 0.001 0.001 

SI>msr 0.002 0.007 0.003 0.003 

cvl'llST 1.5 2.9 4.6 4.1 

RR 

Scnim 

n, 

Median, 

cSD, 

n. 

Median, 

cSD. 

P(n=p) 

P(n<p) 

231 

13 

0.154 

0.079 

RRXL 

232 233 

12 13 

0.258 0.059 

XXXIV 

209 

10 

0.067 

0.010 

234 

13 

0.062 

0.065 0.010 0.019 

0.89 

0.04* 

so .... 0.079 0.065 0.010 0.018 

cv.. 51 25 17 30 

a: O 

b: 0.933 ±0.002 

R2

: 1.000 

<-Current Results-> 

6 6 6 5 

0.264 0.028 0.029 0.033 

0.004 0.001 0.001 0.002 

0.004 0.002 0.001 0.002 

0.001 0.001 0.001 0.001 

0.006 0.002 0.002 0.003 

2.2 8.0 7.5 9.6 

RRXL 

231 232 233 

10 7 9 

0.240 0.027 0.030 

0.025 0.009 0.008 

XXXIV 

209 

6 

0.027 

0.001 

234 

9 

0.030 

0.009 

0.83 

o.oo• 

0.024 0.009 0.008 0.008 

10 32 26 28 

NAV 0.149 0.249 0.057 0.063 <-Assignments-> 0.252 0.02.8 0.030 0.032 

NAU 0.079 0.065 0.010 0.019 0.025 0.009 0.008 0.009 

CV 53 26 18 29 9.9 32 27 28 

xCV 

a: -0.003 ±0.001 

b: 1.114 ±0.008 

R2

: 1.000 

F16
 
Analysis Results Round Robin XL: Sera 231-234 

NIST Data and Value/Uncertainty Assignments 

''Lutein&Zeaxanthin" 

NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

I 

I 

n, 

Mean 

SD 

so,_ 

s0isoN1ST, 

CVNIST, 

n 

Mean 

so ... so. 

so ... 

231 232 233 

0 0 0 

NIST 

6 6 6 

0.408 0.268 0.084 

0.006 0.003 0.003 

0.005 0.008 0.001 

0.021 0.021 0.021 

234 

0 

5 

0.098 

0.004 

0.003 

0.021 

SDwr 0.022 0.023 0.021 0.022 

CVNIST 5.5 8.4 25 22 

RR 

Serum 

n. 

Median., 

eSD1 

P(n=p) 

P(n<p) 

231 

20 

0.355 

0.079 

RRXL 

232 233 

20 20 

0.266 0.<171 

0.085 0.019 

SDw,. 0.075 0.082 

cv...,. 21 31 

0 

0 

XXXIV 

209 

17 

0.094 

0.021 

234 

20 

0.086 

0.017 

0.88 

0.78 

0 

0 

NAV 0.381 0.267 0.081 0.092 

NAU 0.079 0.085 0.021 0.022 

CV 21 32 27 24 

xCV 

231 232 233 234 

0.404 0.267 0.080 0.102 

0.400 0.269 0.086 

0.415 0.278 0.086 0.095 

0.406 0.274 0.082 0.102 

0.411 0.258 0.084 0.091 

0.412 0.264 0.086 0.099 

6 6 6 5 

0.408 0.268 0.084 0.098 

0.006 0.007 0.003 0.005 

0.004 0.003 0.003 0.004 

0.005 0.008 0.001 0.003 

0.007 0.008 0.003 0.005 

1.6 3.1 3.8 5.5 

a:O 

b: 1.101 ±0.047 

R2:0.966 

11 

F17
 
 

Appendix G. “All-Lab Report” for RR40 

The following six pages are the “All-Lab Report” as provided to all participants, with two 

exceptions: 

• the participant identifiers (Lab) have been altered. 

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

The data summary in the “All-Lab Report” has been altered to ensure confidentiality of 

identification codes assigned to laboratories. 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. 

G1
 
Round Robin XL Laboratory Results 

Values in μg/mL 

Retinol Retinyl Palmitate α-Tocopherol γ-Tocopherol

Lab 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BGa 

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-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-EI 

FSV-EL 

FSV-EM 

FSV-FN 

231 232 233 234 

0.291 0.449 0.830 0.517 

0.258 0.388 0.792 0.519 

0.414 0.790 0.493 

0.293 0.454 0.839 0.537 

0.276 0.488 0.803 0.540 

0.329 0.536 0.964 0.600 

0.166 0.261 0.620 0.490 

0.274 0.430 0.770 0.491 

0.285 0.452 0.806 0.527 

0.280 0.446 0.815 0.527 

<0.11 0.229 0.315 0.516 

0.273 0.309 0.478 0.476 

0.251 0.414 0.780 0.502 

0.298 0.441 0.842 0.539 

0.251 0.415 0.758 0.478 

0.291 0.462 0.867 0.548 

0.280 0.410 0.760 0.560 

0.250 0.390 0.720 0.490 

0.297 0.461 0.796 0.572 

0.231 0.394 0.734 0.458 

0.255 0.378 0.725 0.418 

0.252 0.288 0.742 0.517 

0.264 0.529 0.855 0.514 

0.254 0.410 0.667 0.390 

0.235 0.370 0.685 0.425 

0.250 0.387 0.840 0.527 

0.270 0.380 0.631 0.432 

0.277 0.422 0.730 0.518 

0.246 0.421 0.745 0.483 

0.234 0.376 0.653 0.434 

0.213 0.386 0.750 0.443 

0.235 0.467 0.901 0.598 

0.233 0.384 0.744 0.509 

0.263 0.428 0.778 0.481 

0.270 0.430 0.790 0.520 

0.231 0.385 0.779 0.504 

0.268 0.428 0.749 0.474 

0.200 0.450 0.810 0.510 

0.266 0.408 0.770 0.500 

0.293 0.427 0.769 0.483 

0.330 0.460 0.940 0.520 

0.298 0.476 0.915 0.616 

0.269 0.425 0.783 0.504 

0.337 0.457 0.754 0.514 

0.325 0.507 0.948 0.563 

0.223 0.358 0.676 0.404 

0.220 0.380 0.680 0.490 

0.280 0.440 0.770 0.480 

0.278 0.409 0.735 0.525 

231 232 233 234 

0.67 0.97 0.161 0.216 

0.65 0.92 0.140 0.157 

0.85 1.09 0.166 0.159 

0.71 1.47 0.227 0.199 

0.92 1.36 0.232 0.188 

0.69 1.06 0.191 0.155 

0.84 1.32 0.180 0.185 

1.69 2.74 0.375 0.320 

0.14 0.22 0.199 0.178 

0.83 1.23 0.266 0.142 

0.50 0.72 0.163 0.190 

0.82 1.47 0.250 0.180 

1.12 1.22 0.198 0.172 

0.42 0.65 0.118 0.113 

0.87 1.37 0.152 0.155 

δ-Tocopherol

231 232 233 234 

4.72 6.61 7.66 9.68 

4.00 6.80 8.30 9.90 

6.77 8.33 9.76 

5.26 7.48 8.87 10.19 

4.78 7.14 7.50 9.53 

5.06 7.34 8.54 10.24 

5.18 7.10 8.31 10.32 

4.60 6.62 7.82 9.28 

6.02 7.95 9.24 9.22 

4.72 6.73 7.81 9.64 

2.58 4.31 5.17 8.61 

5.50 7.90 7.30 10.90 

4.82 7.48 7.89 9.59 

5.38 7.11 9.26 9.99 

5.07 7.05 8.36 10.45 

5.40 7.40 8.90 11.30 

4.01 5.81 7.15 9.38 

4.08 6.31 7.55 8.60 

4.35 6.06 8.04 9.46 

5.25 6.81 6.97 8.33 

5.16 8.82 9.22 10.11 

5.90 7.30 8.75 10.10 

3.97 5.97 7.02 7.43 

3.88 6.64 7.98 9.68 

4.87 6.78 8.28 9.70 

4.68 6.89 9.00 9.65 

4.93 7.32 8.05 9.97 

4.60 7.80 7.40 9.10 

4.21 6.17 7.14 8.70 

3.91 5.75 7.49 7.83 

5.71 6.28 9.22 8.39 

<4.0 6.63 8.00 10.35 

4.05 6.13 7.10 8.79 

5.22 7.15 7.33 10.08 

5.10 7.10 8.40 10.30 

4.30 6.12 7.00 9.38 

7.06 8.18 9.35 10.16 

5.48 7.03 8.67 9.75 

5.19 6.70 8.19 9.77 

5.00 6.70 9.00 8.80 

4.42 6.61 7.55 9.35 

5.17 6.82 7.52 10.11 

6.14 7.48 8.62 10.17 

4.45 6.62 7.33 7.72 

4.14 6.35 7.26 8.85 

5.29 7.19 7.74 11.47 

n 47 49 49 49 15 15 15 15 44 46 46 46 25 26 26 26 4 3 3 3 

Min 0.166 0.229 0.315 0.390 0.14 0.22 0.118 0.113 2.58 4.31 5.17 7.43 1.00 2.00 0.41 1.73 0.821 0.158 0.171 0.100 

Median	 0.268 0.421 0.770 0.509 0.82 1.22 0.191 0.178 4.90 6.80 7.99 9.68 1.36 2.84 0.76 2.28 1.056 0.174 0.184 0.116 

Max 0.337 0.536 0.964 0.616 1.69 2.74 0.375 0.320 7.06 8.82 9.35 11.47 3.30 3.60 2.80 2.65 1.190 0.222 0.200 0.155 

eSD 0.026 0.047 0.056 0.034 0.15 0.31 0.050 0.024 0.68 0.49 0.87 0.73 0.14 0.29 0.07 0.20 

eCV 10 11 7 7 18 25 26 14 14 7 11 8 10 10 10 9 

231 232 233 234 

1.53 2.88 1.01 2.44 

2.85 0.79 2.41 

1.39 2.87 0.77 2.35 

1.34 2.83 0.73 2.27 

1.33 2.78 0.78 2.31 

1.38 2.29 0.77 2.07 

1.35 2.62 0.70 2.13 

1.65 3.17 0.89 2.12 

1.45 3.00 0.72 2.62 

1.19 2.00 0.61 1.90 

1.30 2.90 0.73 2.21 

1.22 2.85 0.79 2.44 

1.39 2.68 0.74 2.17 

1.48 3.42 0.91 2.30 

3.30 3.60 1.20 2.65 

1.28 2.42 0.68 2.00 

1.00 2.16 0.54 1.73 

1.24 2.44 0.63 2.04 

1.10 3.03 2.80 2.36 

1.07 2.24 0.41 1.87 

1.31 3.14 0.79 2.22 

1.54 2.65 0.93 2.34 

1.51 2.93 0.71 2.51 

1.44 2.59 0.72 2.30 

1.47 3.07 0.82 2.07 

1.36 2.60 0.76 2.29 

231 232 233 234 

1.11 0.16 0.18 0.12 

0.82 0.17 0.17 0.10 

1.00 <0.3 <0.3 <0.3 

1.19 0.22 0.20 0.16 

NISTa
 

NISTb
 

0.251 0.403 0.780 0.485 

0.259 0.421 0.779 0.500 

4.72 6.65 8.00 9.51 

4.74 6.66 7.70 9.84 

1.43 2.71 0.73 2.16 

1.44 2.65 0.73 2.28 

1.14 nd nd nd 

1.02 1.40 0.182 0.151 1.15 0.23 0.24 0.17

NAV
 

NAU
 

0.261 0.417 0.775 0.501 

0.027 0.065 0.065 0.044 

0.82 1.22 0.191 0.178 

0.15 0.31 0.050 0.024 

4.82 6.73 7.92 9.61 

0.69 0.91 0.88 0.77 

1.40 2.76 0.75 2.25 

0.17 0.38 0.11 0.25 

All Lab Report G2	 Page 1 / 6 
Round Robin XL Laboratory Results 

Values in μg/mL 

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

Lab 231 232 233 234 231 232 233 234 231 232 233 234 231 232 233 234 

FSV-BA 0.075 0.254 0.533 0.678 0.074 0.245 0.494 0.626 0.001 0.009 0.039 0.052 0.049 0.011 0.129 0.034 

FSV-BD 0.074 0.217 0.447 0.523
 

FSV-BE
 0.227 0.544 0.663
 

FSV-BF
 0.062 0.253 0.569 0.573 0.036 0.015 0.107 0.023 

FSV-BG 0.068 0.195 0.433 0.625 0.042 0.020 0.081 0.024 

FSV-BGa 0.063 0.196 0.492 0.659 0.037 0.016 0.082 0.047 

FSV-BH 0.070 0.213 0.446 0.603 0.070 0.213 0.430 0.570 <0.01 <0.01 0.016 0.033 0.053 0.013 0.107 0.029 

FSV-BI 0.066 0.211 0.457 0.562 0.045 0.012 0.103 0.025 

FSV-BJ 0.076 0.219 0.463 0.610 0.068 0.027 0.173 0.046 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.078 0.268 0.608 0.706 0.065 0.248 0.569 0.637 nq nq 0.012 0.041 0.048 0.015 0.111 0.028 

FSV-BO 0.064 0.211 0.484 0.533 0.037 0.014 0.097 0.027 

FSV-BP 0.068 0.296 0.651 0.614 0.056 0.022 0.151 0.031 

FSV-BQ 

FSV-BR 

FSV-BS 0.060 0.220 0.410 0.570 0.030 nq 0.070 0.020 

FSV-BU 0.077 0.226 0.496 0.616 0.056 0.014 0.107 0.029 

FSV-BV 0.101 0.280 0.544 0.551 0.037 0.011 0.087 0.021 

FSV-BW 0.125 0.393 0.778 0.968 0.066 0.016 0.144 0.021 

FSV-BX 0.207 0.602 0.103 0.053 0.079 0.077 0.146 0.045 

FSV-BY 0.083 0.295 0.535 0.650 0.073 0.266 0.489 0.569 0.011 0.030 0.046 0.081 0.044 0.027 0.093 0.038 

FSV-BZ 0.040 0.136 0.334 0.548 0.040 0.136 0.330 0.511 nd nd 0.004 0.037 0.039 0.027 0.072 0.036 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 0.068 0.216 0.471 0.530 0.036 0.009 0.079 0.022 

FSV-CE 0.082 0.243 0.567 0.544
 

FSV-CF
 

FSV-CH
 0.047 0.196 0.399 0.561 0.028 0.006 0.079 0.020 

FSV-CK 0.083 0.213 0.494 0.548 0.059 0.105 0.123 0.038 

FSV-CL 0.065 0.209 0.494 0.587 0.059 0.012 0.119 0.029 

FSV-CM 

FSV-CN 0.047 0.160 0.438 0.544 0.033 nq 0.078 0.013 

FSV-CQ 0.356 0.572 0.457 0.475
 

FSV-CR
 

FSV-CS
 0.092 0.276 0.569 0.660 0.083 0.255 0.523 0.591 0.009 0.021 0.046 0.069 0.062 0.016 0.133 0.033 

FSV-CU 

FSV-CX 0.070 0.340 0.820 0.860 0.040 0.010 0.110 0.040 

FSV-DA 0.072 0.216 0.498 0.620 0.066 0.200 0.457 0.578 0.006 0.016 0.041 0.042 0.051 0.021 0.093 0.023 

FSV-DB 0.055 0.167 0.378 0.542 

FSV-DJ
 

FSV-DK
 0.091 0.263 0.591 0.790 0.053 0.017 0.116 0.031 

FSV-DP 

FSV-DQ 0.184 0.161 0.138 0.620 0.012 0.015 0.037 0.030 

FSV-DR 0.098 0.320 0.661 0.690
 

FSV-EI
 0.082 0.290 0.660 0.502 0.056 0.020 0.125 0.024 

FSV-EL
 

FSV-EM
 

FSV-FN
 

n 30 31 31 31 10 10 10 10 4 4 7 7 28 26 28 28 

Min 0.040 0.136 0.103 0.053 0.040 0.136 0.330 0.502 0.001 0.009 0.004 0.033 0.012 0.006 0.037 0.013 

Median 0.075 0.226 0.494 0.610 0.068 0.233 0.473 0.570 0.008 0.019 0.039 0.042 0.047 0.016 0.107 0.029 

Max 0.356 0.602 0.820 0.968 0.083 0.290 0.660 0.637 0.011 0.030 0.046 0.081 0.079 0.105 0.173 0.047 

eSD 0.017 0.050 0.086 0.083 0.009 0.037 0.062 0.029 0.022 0.016 0.014 0.006 0.031 0.009 

eCV 22 22 17 14 14 16 13 5 56 38 30 41 29 29 

NISTa 

NISTb 

NAV
 

NAU
 

0.074 0.230 0.447 0.642 0.070 0.206 0.373 0.542 

0.077 0.224 0.434 0.638 0.065 0.202 0.399 0.586 

0.075 0.227 0.467 0.624 0.068 0.218 0.429 0.566 

0.017 0.050 0.094 0.086 0.010 0.042 0.088 0.059 

0.004 0.025 0.074 0.099 0.051 0.026 0.100 0.038 

0.011 0.021 0.036 0.052 0.052 0.022 0.117 0.046 

0.047 0.059 0.049 0.020 0.108 0.035 

0.042 0.050 0.015 0.009 0.031 0.013 

All Lab Report G3 Page 2 / 6 
Round Robin XL Laboratory Results 

Values in μg/mL 

Total Lycopene trans-Lycopene β-Cryptoxanthin α-Cryptoxanthin

Lab 231 232 233 234 231 232 233 234 

0.128 0.177 0.132 0.185 

0.102 0.128 0.086 0.148 

0.120 0.196 0.134 0.165 

0.107 0.169 0.114 0.155 

0.078 0.104 0.082 0.106 

0.126 0.159 0.112 0.176 

0.108 0.111 0.109 0.111 

231 232 233 234 

0.052 0.179 0.365 0.046 

0.039 0.134 0.256 0.026 

0.036 0.122 0.285 0.027 

0.038 0.013 0.028 0.021 

0.053 0.141 0.292 0.046 

0.050 0.157 0.355 0.039 

0.043 0.146 0.321 0.032 

0.044 0.117 0.260 0.033 

0.071 0.116 0.236 0.068 

0.050 0.160 0.300 0.040 

0.045 0.127 0.271 0.035 

0.075 0.141 0.307 0.027 

0.041 0.145 0.259 0.030 

0.045 0.123 0.270 0.038 

0.050 0.123 0.268 0.042 

0.041 0.083 0.177 0.028 

0.033 0.119 0.265 0.025 

0.044 0.131 0.251 0.031 

0.080 0.280 0.630 0.060 

0.047 0.131 0.265 0.038 

0.052 0.146 0.341 0.047 

0.078 0.181 0.184 0.047 

0.047 0.171 0.323 0.036 

231 232 233 234 

0.008 0.009 0.017 0.013 

0.018 0.019 0.024 0.034 

0.012 0.010 0.018 0.013 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BGa 

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-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-EI 

FSV-EL 

FSV-EM 

FSV-FN 

n 

Min 

Median 

Max 

eSD 

eCV 

NISTa 

NISTb 

NAV 

NAU 

All Lab Report 

0.158 0.192 0.144 0.195 

0.205 0.262 0.200 0.264 

0.203 0.219 0.164 0.278 

0.173 0.190 0.184 0.334 

0.241 0.261 0.224 0.298 

0.196 0.241 0.187 0.279 

0.215 0.322 0.220 0.328 

0.245 0.312 0.257 0.322 

0.228 0.251 0.286 0.341 

0.086 0.283 0.322 0.429 

0.180 0.190 0.120 0.220 

0.269 0.265 0.209 0.324 

0.191 0.254 0.198 0.234 

0.480 0.563 0.398 0.598 

0.192 0.271 0.995 0.726 

0.190 0.275 0.204 0.263 

0.195 0.220 0.190 0.242 

0.228 0.246 0.199 0.268 

0.085 0.125 0.077 0.144 

0.153 0.168 0.155 0.218 

0.180 0.184 0.125 0.183 

0.150 0.115 0.087 0.218 

0.271 0.274 0.256 0.328 

0.140 0.220 0.170 0.230 

0.259 0.268 0.209 0.337 

0.170 0.199 0.152 0.320 

0.332 0.375 0.310 0.478 

0.177 0.221 0.184 0.265 

28 28 28 28 

0.085 0.115 0.077 0.144 

0.194 0.249 0.199 0.279 

0.480 0.563 0.995 0.726 

0.044 0.055 0.052 0.072 

23 22 26 26 

0.236 0.242 0.209 0.333 

0.215 0.245 0.204 0.304 

0.058 0.061 0.053 0.080 

7 7 7 7 

0.078 0.104 0.082 0.106 

0.108 0.159 0.112 0.155 

0.128 0.196 0.134 0.185 

0.014 0.040 0.019 0.030 

13 25 17 20 

0.099 0.120 0.094 0.149 

0.103 0.140 0.103 0.151 

0.023 0.048 0.026 0.032 

G4
 

23 23 23 23 

0.033 0.013 0.028 0.021 

0.047 0.134 0.270 0.036 

0.080 0.280 0.630 0.068 

0.007 0.022 0.042 0.011 

16 16 16 31 

0.035 0.102 0.241 0.027 

0.041 0.118 0.256 0.031 

0.015 0.039 0.062 0.013 

3 3 3 3 

0.008 0.009 0.017 0.013 

0.012 0.010 0.018 0.013 

0.018 0.019 0.024 0.034 

Page 3 / 6 
Round Robin XL Laboratory Results 

Values in μg/mL 

Lutein Zeaxanthin Lutein&Zeaxanthin 

Lab 231 232 233 234 231 232 233 234 231 232 233 234 

FSV-BA 0.683 0.529 0.152 0.124 

FSV-BD 0.144 0.361 0.059 0.059 0.244 0.035 0.031 0.023 0.388 0.396 0.090 0.082 

FSV-BE 

FSV-BF 0.294 0.236 0.071 0.086 

FSV-BG 0.154 0.285 0.048 0.055 0.098 0.019 0.011 0.030 0.252 0.304 0.059 0.085 

FSV-BGa 

FSV-BH 0.110 0.202 0.063 0.043 0.230 <0.02 <0.02 <0.02 0.340 0.202 0.063 0.043 

FSV-BI 0.116 0.212 0.040 0.042 0.236 0.024 0.025 0.015 0.352 0.236 0.065 0.057 

FSV-BJ 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.124 0.244 0.038 0.043 0.243 0.027 0.019 0.019 0.367 0.271 0.057 0.062 

FSV-BO 0.219 0.200 0.050 0.051 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BS 0.430 0.260 0.060 0.100 

FSV-BU 0.594 0.295 0.087 0.110 

FSV-BV 0.305 0.236 0.071 0.076 

FSV-BW 

FSV-BX 0.152 0.224 0.063 0.077 0.179 0.020 0.013 0.014 0.331 0.244 0.076 0.091 

FSV-BY 0.155 0.362 0.057 0.062 0.202 nq 0.022 0.020 0.357 0.362 0.079 0.082 

FSV-BZ 0.238 0.231 0.080 0.087 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 0.312 0.207 0.064 0.080 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CK 0.346 0.257 0.087 0.100 

FSV-CL 0.226 0.177 0.065 0.073 

FSV-CM 

FSV-CN 0.109 nd 0.057 0.058 0.222 nd 0.037 0.034 0.331 0.213 0.094 0.092 

FSV-CQ 

FSV-CR 

FSV-CS 0.375 0.315 0.082 0.086 

FSV-CU 

FSV-CX 0.230 0.390 0.100 0.080 0.270 0.040 0.030 0.030 0.500 0.430 0.130 0.110 

FSV-DA 0.159 0.260 0.059 0.071 0.302 0.030 0.033 0.036 0.461 0.290 0.092 0.107 

FSV-DB 0.319 0.209 0.075 0.079 

FSV-DJ 

FSV-DK 0.318 0.235 0.067 0.084 

FSV-DP 

FSV-DQ 0.107 0.141 0.133 0.093 

FSV-DR 

FSV-EI 0.139 0.309 0.053 0.062 0.262 0.060 0.037 0.036 0.401 0.369 0.090 0.098 

FSV-EL 

FSV-EM 

FSV-FN 

n 14 13 14 14 11 8 10 10 22 22 22 22 

Min 0.109 0.202 0.038 0.042 0.098 0.019 0.011 0.014 0.107 0.141 0.050 0.043 

Median 0.153 0.257 0.059 0.062 0.236 0.029 0.028 0.027 0.346 0.252 0.076 0.086 

Max 0.346 0.390 0.100 0.100 0.302 0.060 0.037 0.036 0.683 0.529 0.152 0.124 

eSD 0.063 0.058 0.009 0.017 0.030 0.010 0.009 0.010 0.068 0.076 0.019 0.015 

eCV 41 23 15 28 13 35 34 39 20 30 25 17 

NISTa 

NISTb 

NAV
 

NAU
 

0.144 0.240 0.055 0.065 0.264 0.028 0.029 0.033 0.408 0.268 0.084 0.098 

0.149 0.248 0.057 0.064 

0.063 0.059 0.013 0.018 

0.250 0.028 0.028 0.030 

0.075 0.010 0.010 0.011 

0.377 

0.088 

0.260 

0.077 

0.080 

0.020 

0.092 

0.021 

All Lab Report G5 Page 4 / 6 
Round Robin XL Laboratory Results 

Analytes Reported By One Laboratory 

Values in μg/mL 

Term 

n 

Min 

Median 

Max 

eSD 

eCV 

NAV 

NAU 

nd 

nq 

<x 

italics 

Analyte Code 231 232 233 234 

Coenzyme Q10 FSV-CH 0.247 0.216 0.166 1.014 

Total Carotenoids FSV-EM 0.800 0.780 1.100 1.150 

trans-α-Carotene NISTb 0.047 0.016 0.107 0.030 

Legend 

Definition

 Number of (non-NIST) quantitative values reported for this analyte

 Minimum (non-NIST) quantitative value reported

 Median (non-NIST) quantitative value reported

 Maximum (non-NIST) quantitative value reported

 Estimated standard deviation, calculated from the median absolute deviation

 from the median of the non-NIST results

 Coefficient of Variation for (non-NIST) results: 100*eSD/Median

 NIST Assigned Value, our estimate of the "true" analyte concentration

 NIST Assigned Uncertainty, our estimate of the total (serum hetergeniety and

 inter- and intra-laboratory) standard deviation

 For details on how we assign these quantities, see the "Analysis of Results."

 Not detected (i.e., no detectable peak for analyte)

 Detected but not quantitatively determined

 Concentration less than x, the limit of detection 

 Not explicitly reported but calculated by NIST from reported values

All Lab Report G6 Page 5 / 6 
All Lab Report 

Round Robin XL Laboratory Results 

Comparability Summary 

Lab 

FSV-BA 

FSV-BD 

FSV-BE 

FSV-BF 

FSV-BG 

FSV-BGa 

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-BU 

FSV-BV 

FSV-BW 

FSV-BX 

FSV-BY 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CH 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-EI 

FSV-EL 

FSV-EM 

FSV-FN 

NISTa 

NISTb 

n 

Lab 

1 57 65 68 64 75 

2 35 33 18 21 17 

3 6 2 7 3 8

4 2 0 7 12 0 

R aT gT bC tbC 

2 3 2 2 2 

1 1 1 1 

3 1 1 1 

2 1 1 1 

3 3 

1 2 2 

2 2 1 2 

1 1 4 

1 1 1 1 

2 1 3 1 1 

4 1 2 1 1 

2 3 2 1 

2 2 1 4 

2 4 2 3 

1 

4 4 

1 2 2 1 

1 1

1 2

2 2 3 2

3 2 4 1

3 4 1 4 

2 2 

1 2 2 

1 1 2 2 2 

3 3 1 3 

1 1 

2 2 2 

2 

2 3 

3 2 

4 2 

1 1 

3 2 1 2 

3 1 2 2 

2 1 2 

2 2 2 1 

1 1 2 1 1 

1 

2 

2 2 1 2 

2 2 3 2 

1 1 

2 1 2 4 

1 2 

2 2 2 

3 2 2 

3 1 1 4 

1 1 

1 3 1 

1 1 2 

1 1 1 1 1 

1 1 1 1 1 

49 46 26 31 10 

% Observed 

Label 

Lab

R 

aT 

gT 

bC 

tbC 

n 

Definition

 laboratory number 

 "Standard Score" for Retinol 

 "Standard Score" for α-Tocopherol

 "Standard Score" for γ-Tocopherol

 "Standard Score" for Total β-Carotene

 "Standard Score" for trans-β-Carotene

number of (non-NIST) laboratories providing data for this analyte 

"Standard Score" 

Given that our knowledge of the shape, location, and width of the measurement 

distributions is approximate and that a limited number of labs are involved, we 

summarize comparability with the following four-level "Standard Score" (StS)... 

StS 

1 

2 

3 

4 

where: 

StV 

NAV 

NAU 

t (1-α,n-1)

Expected 

68.2 % 

27.3 % 

 4.3 % 

0.3 % 

Definition

 All StV within ±t (1-0.683,n-1) 

 All StV within ±t (1-0.954,n-1) 

 All StV within ±t (1-0.997,n-1) 

 At least one StV > ±t (1-0.997,n-1) 

{i.e., ±1 SD} 

{i.e., ±2 SD} 

{i.e., ±3 SD} 

{i.e., >3 SD} 

 Standardized Value, the distance in standard deviation units your

 value is from the "true" concentration: StV = (your value - NAV) / NAU 

 NIST Assigned Value, our estimate of the "true" analyte concentration

 NIST Assigned Uncertainty, our estimate of the total measurement

 standard deviation (serum heterogeniety, analytical repeatibility,

 and among-laboratory reproducibility)

 Two-tailed Student's t for coverage of ±1, ±2, and ±3 NAU about

 NAV, assuming a normal population of size n 

These are the observed and normal-population-expected proportions of 

each Standard Score (StS), based upon each laboratory's largest StV for 

the four sera.

G7 Page 6 / 6 
 

 

 

 

Appendix H. Representative “Individualized Report” for RR40 

Each participant in RR40 received an “Individualized Report” reflecting their reported 

results. Each report included a detailed analysis of the results they reported for the 

following analytes: 

• Retinol 

• Retinol palmitate 

• α-Tocopherol 

• γ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total α-Carotene 

• Total Lycopene 

• β-Cryptoxanthin 

• Lutein 

• Lutein & Zeaxanthin 

The software used to generate the original RR40 “Individualized Reports” is no longer 

available and we do not have a hardcopy of the report as it was sent to any participant or 

NIST analyst. The following 11 pages were produced for participant FSV-BA using a 

descendant of the 1997 software. Three of the graphical tools used in the original reports 

(“Boxplot Comparisons”, “Z-Score Concordance”, and “NIST Assigned Values Vs 

Laboratory Values”) have been retained and display the same information in much the 

same manner as in the original. However, the original report presented the same type of 

information for a number of analytes together on one or two pages rather than presenting 

all information for a given analyte on a single page. The modern software does not 

provide the “% RSD Bias and Precision History” table or the “% Difference” plots. 

H1
 
 Set 1 of 51 

Individualized Round Robin XL Report: FSV-BA 

Summary 

Serum 231 Serum 232 Serum 233 Serum 234 

Analyte You NAV n You NAV n You NAV n You NAV n 

Retinol 0.291 0.261 47 0.449 0.417 49 0.830 0.775 49 0.517 0.501 49 

Retinyl Palmitate 0.668 0.820 15 0.973 1.220 15 0.161 0.191 15 0.216 0.178 15 

α-Tocopherol 4.72 4.82 44 6.6 6.7 46 7.7 7.9 46 9.68 9.61 46 

γ-Tocopherol 1.53 1.40 25 2.88 2.76 26 1.01 0.75 26 2.44 2.25 26 

Total β-Carotene 0.075 0.075 30 0.254 0.227 31 0.533 0.467 31 0.678 0.624 31 

trans-β-Carotene 0.074 0.068 10 0.245 0.218 10 0.494 0.429 10 0.626 0.566 10 

Total cis-β-Carotene 0.001 4 0.009 4 0.039 0.047 7 0.052 0.059 7 

Total α-Carotene 0.049 0.049 28 0.011 0.020 26 0.129 0.108 28 0.034 0.035 28 

trans-Lycopene 0.128 0.103 7 0.177 0.140 7 0.132 0.103 7 0.185 0.151 7 

β-Cryptoxanthin 0.052 0.041 23 0.179 0.118 23 0.365 0.256 23 0.046 0.031 23 

Lutein&Zeaxanthin 0.683 0.377 22 0.529 0.260 22 0.152 0.080 22 0.124 0.092 22 

You : Your reported values for the listed analytes (micrograms/milliliter)
 

NAV : NIST Assigned Values, here equal to this RR's median
 

n : Number of non-NIST laboratories reporting quantitative values for this analyte in this serum 

Please check our records against your records. Send corrections and/or updates to... 

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology Tel: (301) 975-3935 

100 Bureau Drive Stop 8392 Fax: (301) 977-0685 

Gaithersburg, MD 20899-8392 USA Email: david.duewer@nist.gov 

Individualized Report Page 1 / 10 

H2
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

Retinol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 2 / 10 

H3
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

Retinyl Palmitate, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 3 / 10 

H4
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

α-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 4 / 10 

H5
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

γ-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 5 / 10 

H6
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

Total β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 6 / 10 

H7
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

trans-β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 7 / 10 

H8
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

Total α-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 8 / 10 

H9
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

Total β-Cryptoxanthin, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 9 / 10 

H10
 
 

 

 

 Set 1 of 51 

Individualized RR XL Report: FSV-BA 

Total Lutein&Zeaxanthin, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

231232233201209234 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

Lyophilized, prepared from a "low" single donor pool augmented with many #231 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #232 New anayltes to ≈50% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #233 New anayltes to ≈90% of normal population level. 

#234 Lyophilized, multi-donor, native. This is the Mid level of SRM 968b. RR32 #201, RR34 #209 

Individualized Report Page 10 / 10 

H11
 
 

 

Appendix I. Shipping Package Inserts for RR41 

The following two items were included in each package shipped to an RR41 participant: 

• Cover letter 

• Datasheet 

The cover letter and datasheet were enclosed in a sealed waterproof bag along with the 

samples themselves. 

I1
 
July 7, 1997 

Dear Colleague: 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg, Maryland 20899-

Enclosed is the set of samples for the second quality assurance round robin exercise (Round 

Ro bin XLI) for FY97. You will find one vial of each of four lyophilized serum samples 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. If an obtained value is below your limit of 

quantitation, please indicate this result on the form by using NQ (Not Quantitated). For analytes 

not measured, please leave a blank. Results are due to NIST by September 19, 1997. Results 

received two weeks after the due date will not be included in the summary report for this round 

robin study. Written feedback concerning the study will be provided around October 27, 1997. 

Samples should be reconstituted with 1.0 mL ofHPLC-grade water or equivalent. We 

recommend that dissolution be facilitated with 3 to 5 min 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 that 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 LC systems creating analytical problems.) Pipette a known volume of serum 

from the vial for analysis. (The final volume of the reconstituted sample is greater than 1.0 mL.) 

For consistency, we request that laboratories use the following absorptivities (E 1 % cm) in 

ethanol: retinol, 1850 at 325 nm; retinyl palmitate, 975 at 325 nm; a-tocopherol, 75.8 at 292 

nm; y-tocopherol, 91.4 at 298 nm; a-carotene, 2800 at 444 nm (in hexane); ~-carotene, 2560 at 

450 nm (in ethanol), 2592 at 452 nm (in hexane); lycopene, 3450 at 4 72 nm (in hexane). 

Please mail or fax your results for Round Robin XLI to: 

Micronutrients Measurement Quality Assurance Program 

NIST 

Bldg.222, Rm.B208 

Gaithersburg, MD 20899 

Fax: (301) 977-0685 

If you have questions regarding this round robin exercise, please call me at (301) 975-3120; 

e-mail me at jeanice.brownthomas@nist.gov; or mail/fax queries to the above address. 

Enclosures 

cc: S. Wise 

I2
 
 

 

NIST/NCI
 

Micronutrients Measurement Quality Assurance Program
 

Round Robin XLI Results from Laboratory #_____ 

Serum 

Analyte 235 236 237 238 Units* 

retinol 

retinyl palmitate 

α-tocopherol 

γ-tocopherol 

δ-tocopherol 

total β-carotene 

trans-β-carotene 

total cis-β-carotene 

total α-carotene 

trans-α-carotene 

total lycopene 

trans-lycopene 

β-cryptoxanthin 

lutein 

zeaxanthin 

lutein&zeaxanthin 

Other Analytes?
 

* We prefer mg/mL 

Today's Date: 

Comments? 

Mail: MMQAP, 222/B208 

NIST Please return results on-or-before Fax: 301-977-0685 

Gaithersburg, MD 20899 September 22, 1997 Email: David.Duewer@NIST.gov 

I3
 
Appendix J. Final Report for RR41

The following ten pages are the final report as provided to all participants: 

•	 Cover letter 

•	 A “Report of Analysis” that: 

o	 describes the nature of the test samples and details any previous distributions 

o	 summarizes aspects of the study that we believe may be of interest to the 

participants 

o	 details the analysis of the NIST results 

•	 A description of the contents of the “All-Lab” report 

J1
 
November 13, 1997 

Dear Colleague: 

UNITED STATES DEPARTMENT OF COMMERCE 

National Institute of Standards and Technology 

Gaithersburg. Maryland 20899-0001 

This report summarizes both overall and individual laboratory performance for the three round 

robin exercises conducted during 1997. Included in this report are: tabular summaries of data for 

Round Robins (RR) XXXIX, XL, and XU; a graphical summary of the interlaboratory median 

vs. individualized laboratory data for retinol, a- and y-tocopherol, and total and trans-Pcarotene; percent bias charts for retinol, a- and y-tocopherol, and trans- and total P-carotene; and 

a summary of individual laboratory performance for the past three years. Tabular data only are 

provided for a-carotene, P-cryptoxanthin, lutein, lycopene, retinyl palrnitate, and zeaxanthin. 

Over the past three years the overall interlaboratory precision has remained at an average 

estimated coefficient of variation ( eCV) of <10% for retinol and a-tocopherol measurements and 

approximately 21 % for P-carotene during the same period of time. The eCV for y-tocopherol 

has remained at about 10% over the past three years. 

A special "Standard Reference Material (SRM) 968b Report" is also enclosed as our "gift" to 

you for supporting our efforts to create a renewal material of the SRM. One of the three 

components of SRM 968b was distributed in each of the round robin exercises during the 1997 

Quality Assurance (QA) Program. This report summarizes your results, the all-participant 

distributions, and the certified or noncertified values for these materials. 

Serum 227 (the high level of SRM 968b) from RRXXXIX (Sera 227-230) was previously 

distributed as Sera 202 in RRXXXII and 210 in RRXXXIV. No significant changes in stability 

were observed. Serum 228 was previously distributed as blind duplicates (Sera 223 and 225) in 

RRXXXVIII. This material was reanalyzed to determine long-term within-laboratory 

measurement precision and among-laboratory measurement concordance. Sera 229 and 230 

were new sera augmented with many of the commonly reported analytes (i.e., retinol, 

o-, y-, and a-tocopherol, lutein, and zeaxanthin. 

RRXL (Sera 231-234) consisted of three new sera and the mid-level SRM 968b (Serum 234) 

which was previously distributed as Sera 201and209. Sera 231-233 were prepared from a 

serum pool as models for the proposed renewal material SRM 968c. The overall laboratory 

performance for retinol, y- and a-tocopherol, and P-carotene for this exercise was comparable to 

that of the overall interlaboratory performance over the past three years. 

The experimental design for Round Robin XLI (Sera 235-238) is summarized below. The four 

serum samples addressed the following issues: 

J2
 
•Serum and Measurement Stability. Serum 235 is the low-level component of SRM 968b, 

Fat-Soluble Vitamins and Cholesterol in Human Serum. It was previously distributed as Sera 

200 (RRXXXII) and 207 (RRXXXIV). Reanalysis of such well-characterized samples 

documents the long-term stability of both materials and measurement systems. No statistically 

significant changes were observed in this material. 

• Analyte augmentation techniques. Sera 236, 237, and 238 were again prepared as models for 

the high-, mid-, and low-level sera of the proposed renewal material SRM 968c. We intend to 

have the three "major" analytes (retinol, a-tocopherol, and P-carotene) at the same relative levels 

in SRM 968b, while having the "minor" analytes ( a-carotene, lycopene, P-cryptoxanthin, lutein, 

and zeaxanthin) at different relative levels in the three sera. This design will provide significant 

added value to laboratories interested in carotenoid speciation. We were successful at achieving 

our target levels in the high- and mid-level samples (Sera 236 and 237, respectively). However, 

the augmentation technique did not work as well for Serum 238. Due to extreme difficulties in 

reconstituting this serum sample, results for Serum 238 were not used in the interlaboratory data 

analyses. 

•Measurement Precision and Concordance. We have modified the "NIST assigned value 

versus your value scatter plots" on page 6 of your "Individualized Data" Report to better 

represent what we expect the measurement uncertainties to be. The plots now present ±1 eSD 

and ±3 eSD contours, instead of± 15% and ±50% measurement intervals. 

Data for evaluating your laboratory's performance in Round Robin XLI are provided in the 

comparability summary on page 6 of the "All Lab" Report. The criteria used to summarize 

laboratory performance are as follows: results rated 1 (within± 1 SD of the assigned value) 

indicate EXCEPTIONAL performance, those rated 2 (within± 2 SD) indicate ACCEPTABLE 

performance, a rating of 3 (within ± 3 SD of the assigned value) is MARGINAL performance, 

and 4 (>3 SD from the assigned value) indicates POOR performance relative to the current 

state-of-the-practice for these measurements. 

If you have concerns regarding your laboratory performance or were rated "POOR" based on the 

criteria stated above, we suggest that you obtain a unit of SRM 968b, Fat-Soluble Vitamins and 

Cholesterol in Human Serum, and analyze all three levels. If with minor method modifications, 

your measured values do not agree with the certified values, we suggest that you contact us for 

consultation. 

We anticipate that the 1998 QA Program will consist of three round robin exercises for the 

analysis of fat-soluble vitamins and carotenoids in serum and one exercise for the analysis of 

ascorbic acid in serum. The first set of samples for the fat-soluble vitamins in serum analysis for 

FY 98 will be distributed during the week of February 9. Results are due by April 3; written 

feedback will be provided to labs around April 30. The second set of samples will be shipped the 

week of May 4 with results due by June 26 and feedback to labs by July 31. The third set of 

samples will be shipped the week of August 10. Results will be due by September 25. Feedback 

will be provided to the laboratories around October 30. 

J3
 
The first set of samples for the measurement of ascorbic acid in serum will be distributed in early 

March 1998. This round robin study is being coordinated by Dr. Sam Margolis (301/975-3137). 

The Fat-Soluble Vitamins and Carotenoid Analysis Tutorial session was held on October 27 at 

NIST. The session was well-attended and provided a great opportunity for new laboratories to 

discuss in detail their measurement techniques. 

Certificates of participation in the FY 97 QA Program will be distributed in January 1998. If you 

have any questions, please feel free to contact me at: 301/975-3120; fax: 301/977-0685; oremail: jeanice.brownthomas@nist.gov. 

· ce Brown Thomas 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

cc: W.E. May 

S. A. Wise 

J4
 
Analysis of Results Round Robin XU: Sera 235-238 Page 1 

Analysis of N2M2QAP Round Robin XLI Results: Sera 235 to 238 

Background: Four samples were distributed in RR41 

Serum 235: the "low level" component of SRM• 968b: Fat-Soluble Vitamins and Cholesterol 

in Human Serum. It was previously distributed as Serum 200 in RR32 (9194) and Serum 207 

in RR34 (6195). 

Sera 236-238: experimental sera, prepared from a single "low" serum pool and augmented 

with the various analytes to (try to) hit 10%, 50%, and 90% population levels. The organic 

solvent-free (HDL, LDL) liposome technique suggested by the RR40 results was used in the 

preparation of all three sera. 

Qualitative Results: The following observations were noted in the RR41 reports: 

Nearly everyone reported that Serum 238 did not reconstitute, often describing a "large 

viscous globule" remaining in the vial. 

Action: Sorry, our mistake and Serum 238 should not have been shipped. We will 

confirm the "reconstitutability" of all new sera prior to shipping. 

No data for Serum 238 will be used in any analysis that reflects on your 

laboratory's performance. The data is of interest to us from the "what does a 

known heterogeneous material look like?" standpoint, so we do report the allparticipant boxplots on pages 2 and 3. (We echo your data for Serum 238 on page 

1 of the individualized report, but flag them as "non-quantitative values".) 

We tried to notify all of you about this problem as soon as it was drawn to our 

attention. We thank all of you who provided us information on this material! 

Note: If you did NOT observe a reconstitution problem with Serum 238, you probably 

SHOULD have. You may want to review your sample-evaluation procedures. 

A few participants noted small amounts of suspended solid in Sera 237 and/or 236. 

Action: We are continuing our analyte augmentation research. We will attempt to reduce 

or eliminate this problem. We will check all new sera for the presence of 

suspended solids on reconstitution. 

Quantitative Results The following NIST Data and Value/Uncertainty Assignments table 

presents all NIST data, summary statistics for the NIST data, summary results for RR41, and 

the NIST assigned values and uncertainties. The entries are defined as follows: 

Individual NIST Analyst Data and Summazy Statistics 

A: 1 to C:2 two aliquots ("1" and "2") of three vials (A, B, and C) of each serum were 

extracted and analyzed. Each analyst analyzed a separate set of three vials. 

n" number of quantitative values for this analyte for this serum for this analyst 

Mean" arithmetic average 

SD" simple standard deviation 

SDrepx within-vial pooled standard deviation, reflecting variation in extraction, 

chromatography, peak integration, etc. 

J5
 
Analysis of Results Round Robin XLI: Sera 235-238 

SD11eu among-sample standard deviation, reflecting heterogeneity in preparing and 

reconstituting the serum samples 

SDNISTx ~SD~ +SD~ , total standard deviation. This value is ~ SDx• as sample 

replicates reduce the true degrees of freedom. 

CV NISTx 100 x SD NJSTiMeanx 

NIST Summax:y Statistics Cfor aoalytes re.ported by both NISTl and NIST3l 

n number of quantitative values for this analyte for this serum 

Mean (MeanNIST1 + MeanNIST3)/2 

SDrep within-vial pooled standard deviation 

SDbet among-sample standard deviation 

between-analyst standard deviation. This is the residual standard deviation for 

regression ofNIST3's Meanx values to NISTl 's. The model used to determine 

SDan1 is defmed to the right of this block. Details include: model used, 

parameters and standard errors on the parameters, and R2 • 

SDNIST ~SD!, +SD~ + SD!.i , total standard deviation for NIST analyses. 

CV NIST 100 x SDms/Mean 

Initial Distribution Cif any> Suromazy Statistics 

RR Round Robin in which this Serum was first distributed 

Serum Sample identification number of the initially distributed Serum 

~ number of non-NIST laboratories reporting quantitative values for this analyte 

for this serum in the initial distribution 

MedianP median of the reported values in the initial distribution 

eSDP 0.741 x InterQuartile Range in the initial distribution 

Round Robin XLI Suromazy Statistics 

nn number of non-NIST laboratories reporting quantitative values for this analyte 

for this serum in this Round Robin 

Mediann median of the reported values in this Round Robin 

eSDn 0.741 x InterQuartile Range in this Round Robin 

.· 

Page2 

J6
 
Analysis of Results Round Robin XLI: Sera 235-238 Page 3 

P(n=p) TDIST{ jMediana -MedianPl~na +nP -2 '~+na·2, 2-tail) 

(Cna -l)eSD! +(np-l)eSD:i_l +-1 ) 

\ na np 

This is the approximate probability that the current median is the same as it was 

in its initial distribution. Where the hypothesis that Mediana = Medi~ can be 

rejected with 95% confidence, the P(n=p) value is flagged with an"*". TDIST 

is Excel4hs student's t function. 

( eSD2 ) P(n<p) FDIST --; , Da-1, ~-1 

eSD0 

This represents the approximate probability that the current interlaboratory 

variance is smaller than it was in its initial distribution. Where the hypothesis 

that eSDa < eSDR can be rejected with 95% confidence, the P(n<p) value is 

flagged with an *". FDIST is Excel GD' s F-distribution function. : 

SDlabs ~eSD! - SD~ , the residual non-NIST interlaboratory biases after correction 

for measurement-, sampl~. and NIST-analyst-related sources of variance. When 

SDNIST is greater than eSDa• SDllbl = 0. 

CV labs 100 x SD~edian.i 

NIST Assi&ned Values and Uncertainties 

NA V (Mean + Mediana) / 2, our best guess of the "true" analyte level 

NAU Maximum( 0.05 x NA V, ~sD:asT +SD~ ), our best guess for the "true" 

interlaboratory standard deviation characterizing measurement, sample 

heterogeneity, interanalyst, and interlaboratory sources of variation. When SD1abs 

could not be determined, NAU is estimated as 

Maximum(0.10 x NAV, ~2 SD~ST ). 

CV lOOxNAU /NAV 

xCV CV "expected" for the given NA V analyte level. This calculation is detailed in: 

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. 

J7
 
Analysis of Results Round Robin XLI: Sera 235-238 

Measurement Performance Summary: The following is based on results presented in the 

NIST Data and Value/Uncertainty Assignments table of this report and the "Individualized 

Report" page 2 and 3 summary graphs: 

Serum 235. low-leyel SRM 968b. stability: There is no significant difference in the level or 

measurement variability of any analyte among the three analyses of this material (Sera 200, 

207, and 235). 

Pagc4 

Serum 236 homo&enejty: Although there were a few reports of incomplete dissolution for this 

serum, the observed measurement variabilities were about as expected for homogeneous 

materials. The observed analyte levels were in excellent accord with the design levels. 

Serum 237 homo~enejty: There were several reports of incomplete dissolution for this serum. 

While most analytes were reasonably well behaved, the observed p-carotene level was lower 

than expected and the observed measurement variability was somewhat higher than expected. 

We suspect that some of the high-level augmented analytes are being non-spec,ifically bound 

to various proteins. 

Action: We continue to refine our augmentation techniques. 

Serum 238 hetero&eneity: The analytes in this serum reconstituted quite differentially. The 

median levels and observed variability were only somewhat greater than expected for the 

relatively hydrophilic retinol and 'Y -tocopherol. The carotenoids levels were much lower than 

designed (and the variability greater than expected for those levels). 

Action: We have added an explicit "reconstitutability" requirement to our sample 

preparation QA/QC. We will continue to refine our augmentation techniques. 

Retjnyl palmjtate: The CVs for all sera are greater than 30%. 

Action: The current SRM 968b "certified" retinyl palmitate levels will be downgraded to 

to "non-certified" (or "reference", if we can upgrade the nomenclature!) values. 

If we can get the funding, we will evaluate the various analytical methodologies 

used or proposed for RP analysis. 

Dave Duewer 

Research Chemist 

David.Duewer@NIST.gov 

Marg et Kline 

Research Biologist 

Margaret.Kline® NIST.gov 

J8
 
Analysis Results Round Robin XL: Seta 231-234 s 

NIST Data and Value/Uncertainty Assignments 

A:I 

A:2 

B:I 

B:2 

C:I 

C:2 

n. 

Mean, 

so. 

so_ 

so.a 

235 

0.308 

0.362 

0.293 

0.278 

0.275 

0.293 

6 

0.301 

0.032 

0.024 

0.029 

Retinol 

NIST I 

236 237 238 235 

0.640 0.810 0.254 0.319 

0.599 0.775 0.214 0.308 

0.626 0.923 0.192 0.285 

0.567 0.937 0.221 0.283 

0.538 0.942 0.230 0.295 

0.562 0.913 0.231 0.295 

6 6 6 6 

0.589 0.883 0.224 0.298 

0.040 0.072 0.021 0.014 

0.031 0.019 0.020 0.005 

0.036 0.079 o.ot5 O.oIS 

NIST3 

236 237 238 235 

0.601 0.896 0.227 8.52 

0.613 0.910 0.234 8.70 

0.569 0.908 0.285 7.18 

0.571 0.863 0.279 7.27 

0.596 0.896 0.211 6.44 

0.598 0.890 0.218 7.27 

6 6 6 6 

0.591 0.894 0.242 7.56 

O.ot8 0.017 0.032 0.87 

0.005 0.019 0.005 0.35 

0.019 0.009 0.035 0.92 

a-Tocopherol 

NISTI NIST3 

236 237 238 235 236 237 238 

13.35 20.8 2.8 7.36 11.39 20.3 2.7 

12.62 21.4 2.9 7.36 11.33 20.2 2.7 

12.62 20.4 2.5 6.71 10.96 20.6 2.9 

12.16 21.4 2.9 6.61 10.97 19.6 2.9 

11.39 20.8 3.0 6.87 11.43 20.2 2.4 

11.31 20.5 3.0 6.94 11.56 20.7 2.5 

6 6 6 6 6 6 6 

12.24 20.9 2.9 6.97 11.27 20.3 2.7 

0.79 0.4 0.2 0.32 0.25 0.4 0.2 

0.36 0.5 0.2 0.05 0.06 0.5 0.0 

0.83 0.2 0.1 ·o.3s 0.27 0.2 0.2 

s~. 0.038 o.047 0.081 o.02s 0.016 0.020 0.021 0.036 o.99 o.90 o.6 0.2 o.36 0.28 o.s 0.2 

cvNJST. 12 8.0 9.2 11 S.2 3.3 2.4 IS 13 7.4 2.7 8.0 S.I 2.5 2.4 8.5 

NIST 

n 12 12 12 12 

Mean 0.299 0.590 0.889 0.233 

SD,. 0.017 0.022 0.019 0.015 

so. 0.021 0.026 0.051 . 0.028 

so... 0.000 0.000 . 0.000 0.000 

SDNIST 0.027 0.034 0.055 0.031 

CVNIST 9.1 5.8 6.2 14 

RR XXXIl 

Serum 200 

Op 40 

Medianp 0.300 

eSDp 0.026 

235 

46 

0.284 

0.018 

0.88 

0.98 

RRXLI 

236 237 238 

46 46 38 

0.602 0.872 0.303 

0.044 0.088 0.035 

Ro 

Median0 

eSD0 

P(n=p) 

P(n<p) 

SD..,.. 

cv...,. 

o 0.021 o.069 o.oi5 

0 4.5 7.9 4.8 

NA V 0.291 0.596 0.880 0.268 

NAU 0.027 0.044 0.088 0.035 

CV 9.3 7.3 10 13 

xCV 9.9 8.7 8.9 10 

[41_dll[NISTut 

NIST3=a+b*NISTI 

a: -0.012 ±0.001 

b: 1.025 ±0.001 

R2: 1.000 

<-Current Results-> 

<-Assignments-> 

12 

7.27 

0.25 

0.63 

0.30 

0.75 

10 

XXXII 

200 

42 

7.16 

0.52 

235 

44 

6.91 

0.55 

0.92 

0.38 

0 

0 

7.09 

0.75 

11 

7.9 

NIST 

12 12 

11.76 20.6 

0.26 0.5 

0.57 0.2 

0.30 0.3 

0.69 0.6 

S.9 2.9 

RRXLI 

236 237 

44 44 

11.53 20.0 

0.74 1.2 

0.24 1.0 

2.1 5.0 

11.64 20.3 

0.74 1.2 

6.3 5.7 

7.2 7.7 

12 

2.8 

0.1 

0.4 

0.3 

0.5 

18 

238 

34 

4.1 

1.2 

I.I 

27 

3.4 

1.2 

35 

13 

NIST3=a+b*NISTI 

a: -0.79 ±0.47 

b: 1.01 ±0.03 

R2: 0.998 

_______________ 

XLI: Sera 235-238
­

J9
 
Analysis Results ROUDd Robin XL: Sen 231-234 6 

NIST Data and Value/Uncertainty Assignments 

y-Tocopherol ~ Tocopherol 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean. 

so. 

SD1e11a 

so._ 

235 . 

2.15 

2.18 

1.70 

1.73 

1.67 

1.70 

6 

1.86 

0.24 

0.02 

0.27 

NISTl 

236 237 238 

7.37 l.15 1.17 

1.05 1.12 1.19 

7.18 1.04 1.07 

7.93 1.14 1.08 

6.11 1.18 1.27 

5.79 1.27 1.24 

6 6 6 

6.91 1.15 1.17 

0.81 0.07 0.08 

0.36 0.05 0.02 

0.84 0.07 0.09 

NIST3 

235 236 237 238 

1.66 5.80 1.07 1.02 

1.66 5.78 1.08 1.07 

1.51 5.55 1.08 1.17 

1.51 5.51 1.03 1.16 

1.54 5.68 1.03 0.93 

1.55 5.74 1.06 0.95 

6 6 6 6 

1.57 5.67 1.06 1.05 

0.07 0.12 0.02 0.10 

0.00 0.03 0.02 0.02 

0.08 0.13 0.01 0.11 

SDNJSra 0.27 0.92 0.09 0.09 0.08 0.14 0.03 0.11 

CVNJSTa 15 13 7.5 7.7 5.1 2.4 2.6 11 

n 

Mean 

SD1e11 

SD..., 

SD..i 

12 

1.71 

0.02 

0.15 

0.04 

NIST 

12 12 12 

6.29 1.10 1.11 

0.26 0.04 0.02 

0.44 0.04 0.08 

0.04 0.04 0.04 

s~ 0.15 o.51 0.01 o.09 

CVNIST 9.0 8.1 6.4 8.5 

RR XXXII 

Serum 200 

n, 18 

Median, 1.69 

eSD, 0.23 

n. 

Median. 

eSD0 

P(n=p) 

P(n<p) 

235 

23 

1.70 

0.26 

0.99 

0.33 

so... 0.21 

cv.. 12 

RRXLI 

236 237 238 

23 23 18 

6.28 1.18 1.51 

0.39 0.19 0.31 

0 0.18 0.29 

0 15 19 

NIST3=a+b*NIST1 

a: 0.11 ±0.04 

b: 0.81 ±0.01 

R2: 1.000 

<-Current Results-> 

NISTl NIST3 

235 236 237 238 235 236 237 238 

0.456 0.612 0.613 0.095 0.330 0.543 0.609 

0.418 0.600 0.639 0.101 0.353 0.536 0.609 

0.414 0.549 0.545 0.087 0.315 0.543 0.701 

0.485 0.641 0.567 0.084 0.311 0.517 0.709 

0.367 0.538 0.622 0.085 0.323 0.502 0.556 

0.380 0.504 0.617 0.094 0.326 0.532 0.561 

0 6 6 6 6 6 6 6 

0.420 0.574 0.601 0.091 0.326 0.529 0.624 

0.045 0.052 0.037 0.007 0,015 0.016 0.067 

0.033 0.040 0.014 0.005 0.010 0.016 0.004 

0.041 0.046 0.039 0.006 0.014 O.otl 0.074 

0.052 0.062 0.041 0.008 0.017 0.020 0.075 

12 11 6.9 8.6 5.3 3.8 12 

NIST 

6 12 12 12 

0.091 0.373 0.551 0.612 

0.005 0.024 0.031 0.010 

0.006 0.032 0.031 0.076 

0.049 0.049 0.049 0.049 

0.050 0.064 0.066 0.091 

54 17 12 15 

XXXIl 

~ rj 

235 

5 

0.090 

0.030 

0 

0 

RRXLI 

236 

6 

0.375 

0.052 

0 

0 

237 

6 

0.575 

0.058 

0 

0 

238 

6 

0.915 

0.068 

0 

0 

NIST3=a+b*NIST1 

a: 0.000± 

b: 0.871 ±0.069 

R2: 0.780 

NAV 1.71 6.28 1.14 1.31 <-Assignments-> 0.091 0.374 0.563 0.764 

NAU 0.26 0.51 0.19 0.31 0.050 0.064 0.066 0.091 

CV 15 8.1 17 23 55 17 12 12 

xCV 9.1 7.2 11 10 

(41_dOllNISTUI 

_______________ 

XLI: Sera 235-238
­

J10
 
Analysis Results Round Robin XL: Sera 231-234 

NIST Data and Value/Uncertainty Assignments 

Total p-Carotene trans p.Carotene 

NISTl NIST3 NISTl NIST3 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n, 

Mean1 

so. 

SD,.. 

so .. 

235 236 237 238 

0.256 0.303 0.311 0.048 

0.226 0.310 0.420 0.060 

0.262 0.317 0.273 0.045 

0.242 0.319 0.455 0.049 

0.239 0.290 0.342 0.047 

0.245 0.283 0.392 0.055 

6 6 6 6 

0.245 0.304 0.366 0.051 

0.013 0.015 0.069 0.006 

0.015 0.004 0.089 0.006 

0.006 0.016 0.002 0.004 

235 236 237 238 

0.243 0.254 0.340 0.043 

0.247 0.267 0.332 0.041 

0.228 0.254 0.376 0.047 

0.231 0.258 0.349 0.050 

0.241 0.269 0.414 0.040 

0.234 0.265 0.403 0.043 

6 6 6 6 

0.237 0.261 0.369 0.044 

0.007 0.007 0.034 0.004 

0.004 0.006 0.012 0.002 

0.008 0.006 0.037 0.004 

235 236 237 238 235 236 237 

0.213 0.205 0.308 0.038 0.229 0.239 0.331 

0.217 0.216 0.340 0.048 0.231 0.249 0.325 

0.202 0.211 0.268 0.044 0.213 0.241 0.373 

0.222 0.210 0.325 0.042 0.213 0.238 0.332 

0.204 0.193 0.265 0.041 0.217 0.257 0.399 

0.225 0.197 0.281 0.044 0.222 0.275 0.390 

6 6 6 6 6 6 6 

0.214 0.205 0.298 0.043 0.221 0.250 0.358 

0.009 0.009 0.032 0.003 0.008 0.014 0.033 

0.012 0.005 0.027 0.004 0.002 0.008 0.017 

0.001 0.009 0.026 0.000 Q.009 0.014 0.034 

7 

238 

0.043 

0.041 

0.047 

0.050 

0.040 

0.043 

6 

0.044 

0.004 

0.002 

0.004 

s0msr. 0.016 0.011 0.089 o.007 o.009 o.oos 0.039 o.004 0.012 0.010 o.038 o.004 o.009 0.011 o.038 o.004 

cvNJSr. 6.6 5.5 24 14 3.6 3.1 10 9.9 5.6 5.o 13 10 4.o 6.6 11 9.9 

n 

Mean 

so_ 

so. 

so ... 

12 

0.241 

0.011 

0.007 

0.025 

NIST 

12 12 12 

0.282 0.367 0.047 

0.005 0.064 0.005 

0.019 0.026 0.004 

0.025 0.025 0.025 

SDNJSr 0.028 0.031 0.073 0.026 

CVNJSr 12 11 20 54 

RR XXXII 

Serum 200 

Op 32 

Meclia0p 0.248 

eSD0 0.040 

na 

Mecliana 

eso. 

P(n=p) 

P(n<p) 

235 

27 

0.242 

0.039 

0.97 

0.56 

RRXLI 

236 237 

27 27 

0.280 0.376 

0.038 0.098 

so...,. 0.027 0.021 0.064 

cv.. II 7.4 17 

238 

22 

0.085 

0.025 

0 

0 

a:0.000± 

b: 0.953 ±0.047 

R2: 0.764 

<-Current Results-> 

NA V 0.242 0.281 

NAU 0.039 0.038 

0.372 

0.098 

26 

16 

0.066 <-Assignments-> 

0.026 

CV 

xCV 

16 

17 

13 

17 

39 

25 

NIST 

12 12 12 12 

0.217 0.228 0.328 0.043 

0.008 0.005 0.026 0.003 

0.016 0.013 0.029 0.004 

0.023 0.023 0.023 0.023 

0.029 0.027 0.045 0.023 

13 12 14 54 

XXXII 

200 

8 

0.232 

0.022 

235 

10 

0.228 

0.023 

0.92 

0.49 

0 

0 

RRXLI 

236 

11 

0.260 

0.018 

0 

0 

237 

II 

0.372 

0.030 

0 

0 

0.222 0.244 0.350 

0.029 0.027 0.045 

13 II 13 

9.4 9.3 9.2 

238 

10 

0.080 

0.008 

0 

0 

0.062 

0.023 

38 

13 

a: 0.000± 

b: 1.162 ±0.054 

R2: 0.812 

_______________ 

XLI: Sera 235-238
­

J11
 
Analysis ResullS 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

235 

0 

Round Robin XL: Sera 231-234 

NIST Data and Value/Uncertainty Assignments 

Total a-carotene 

NISTl NIST3 

Total Lycopene 

NIST3 

236 237 238 235 236 237 238 235 236 237 238 

0.155 0.022 0.032 0.203 0.005 0.189 0.43 0.23 O.ot8 

0.161 0.029 0.042 0.198 0.004 0.196 0.48 0.20 0.023 

0.160 0.024 0.039 0.215 0.005 0.190 0.42 0.26 0.021 

0.173 0.028 0.035 0.207 0.006 0.189 0.41 0.23 0.017 

0.162 0.028 0.030 0.223 0.211 0.47 0.26 o.ot5 

0.152 0.028 0.041 0.216 0.005 0.190 0.51 0.26 0.013 

0 6 0 6 6 6 5 6 6 6 6 

0.160 0.027 0.037 0.210 0.005 0.194 0.45 0.24 0.018 

0.007 0.003 0.005 0.009 0.001 0.009 0.04 0.02 0.004 

0.007 0.003 0.006 0.005 0.001 0.009 0.02 0.02 0.003 

0.005 0.001 0.001 0.010 0.001 0.006 0.04 0.02 0.003 

8 

trans-Lycopene 

NIST3 

235 236 237 238 

0.089 0.34 0.143 0.012 

0.088 0.35 0.132 0.014 

0.083 0.31 0.169 0.014 

0.083 0.32 0.141 0.012 

0.091 0.36 0.181 O.ot 1 

0.085 0.39 0.172 O.ot 1 

6 6 6 6 

0.087 0.34 0.156 0.012 

0.003 0.03 0.020 0.001 

0.002 0.01 0.013 0.001 

0.003 0.03 0.020 0.001 

n, 

Mean, 

SD, 

so_ 

so.­

SI>mm 

cvNJST. 

0.009 

5.5 

0.004 0.006 0.011 0.001 0.011 0.04 0.03 0.004 0.004 0.03 0.023 0.002 

13 17 5.1 15 5.5 9.8 12 24 4.5 9.6 15 13 

NIST 

n 6 6 12 5 

Mean i--~~~~~~~~ 0.027 0.037 0.185 0.005 

SD,. 0.004 0.005 0.006 0.001 

SD..., 0.001 0.001 0.010 0.001 

so • .__~~~~~~~~ 

SDNJST 

CVNJST 

0.004 0.005 0.011 0.001 

15 13 6.1 17 

RR XXXII 

Serum 200 

D0 22 

Median0 0.020 

eSD0 0.009 

Da 

Median0 

eSD0 

P(n=p) 

P(n<p) 

235 

23 

0.021 

0.005 

0.95 

0.99 

RRXLI 

236 237 238 

25 26 17 

0.024 0.206 0.011 

0.006 0.047 0.007 

so.... 0.003 0.004 0.046 0.007 

cv.. 14 15 22 67 

<-Current Results -> 

NA V 0.024 0.030 0.196 

NAU 0.005 0.006 0.047 

0.008 <-Assignments-> 

0.007 

CV 20 20 24 93 

xCV 31 29 26 47 

XXXII 

200 

22 

0.179 

0.031 

235 

25 

0.183 

0.043 

0.97 

0.07 

0.042 

23 

0.189 

0.043 

23 

27 

RRXLI 

236 237 238 

26 26 20 

0.48 0.24 0.057 

0.21 0.11 O.ot8 

0.20 0.11 0.017 

43 44 31 

0.47 0.24 0.037 

0.21 0.11 O.ot8 

45 46 48 

23 26 33 

XXXII 

M 

~ 

235 

7 

0.097 

0.012 

O.ot l 

12 

0.092 

0.012 

13 

RRXLI 

236 237 

7 7 

0.47 0.200 

0.20 0.066 

0.20 0.062 

43 31 

0.40 0.178 

0.20 0.066 

51 37 

238 

5 

0.029 

0.010 

0.010 

33 

0.021 

0.010 

47 

_______________ 

XLI: Sera 235-238
­

J12
 
Analysis Results Round Robin XL: Sera 231-234 

NIST Data and Value/Uncertainty Assignments 

A:l 

A:2 

B:l 

B:2 

C:l 

C:2 

n. 

Mean. 

so. 

so...,. 

so._ 

p-Cryptoxanthin 

NIST3 

235 236 237 238 

0.021 0.096 0.345 0.007 

0.022 0.099 0.334 0.008 

0.021 0.093 0.381 0.008 

0.020 0.093 0.333 0.007 

0.022 0.101 0.384 0.006 

0.021 0.100 0.384 0.007 

6 6 6 6 

0.021 0.097 0.360 0.007 

0.001 0.004 0.025 0.001 

0.001 0.001 0.020 0.001 

0.001 0.004 0.022 0.001 

''Lutein" 

NIST3 

235 236 237 

0.060 0.441 0.065 

0.059 0.447 0.073 

0.054 0.412 0.067 

0.051 0.408 0.062 

0.055 0.433 0.065 

0.055 0.433 0.068 

6 6 6 

0.056 0.429 0.067 

0.003 0.016 0.004 

0.001 0.003 0.004 

0.004 0.017 0.002 

238 

0.04 

0.04 

0.05 

0.05 

0.04 

0.04 

6 

0.04 

0.00 

0.00 

0.00 

"Zeaxanthin" 

NIST3 

235 236 237 238 

0.025 0.051 0.062 0.027 

0.023 0.051 0.066 0.025 

0.022 0.049 0.061 0.029 

0.022 0.048 0.059 0.029 

0.026 0.050 0.064 0.029 

0.026 0.050 0.063 0.026 

6 6 6 6 

0.024 0.050 0.063 0.028 

0.002 0.001 0.002 0.002 

0.001 0.000 0.002 0.001 

0.002 0.001 0.002 0.001 

9 

''Lutein&Zeaxanthin" 

NIST3 

235 236 237 238 

0.085 0.492 0.127 0.067 

0.082 0.498 0.139 0.065 

0.076 0.461 0.128 0.076 

0.073 0.456 0.121 0.076 

0.081 0.483 0.129 0.068 

0.081 0.483 0.131 0.063 

6 6 6 6 

0.080 0.479 0.129 0.069 

0.004 0.017 0.006 0.006 

.. 0.002 0.003 0.006 0.002 

0.005 0.019 0.004 0.006 

SDiasr. 0.001 0.004 0.030 0.001 0.004 O.ot8 0.005 0.00 0.002 0.001 0.003 0.002 0.005 0.019 0.007 0.006 

CVNISTa 4.3 4.1 8.4 13 6.8 4.1 6.9 12 9.0 2.7 4.6 7.6 6.2 3.9 5.6 9.1 

n 

Mean 

SD..., 

SD11e1 

SD1111 

SDiasr 

CVNIST 

RR XXXII 

Serum 200 

Do 16 

Median0 0.041 

eSD0 0.016 

n. 

Median. 

eSD. 

P(n=p) 

P(n<p) 

235 

22 

0.026 

0.008 

0.67 

1.00 

RRXLI 

236 237 

23 23 

0.125 0.419 

0.035 0.083 

238 

17 

O.ot8 

0.010 

XXXII 

200 

11 

0.064 

0.014 

235 

12 

0.070 

0.013 

0.87 

0.64 

RRXLI 

236 237 238 

11 12 11 

0.502 0.079 0.08 

0.049 0.030 0.07 

XXXII 

200 

6 

0.020 

0.005 

235 

9 

0.023 

0.008 

0.83 

0.14 

RRXLI 

236 237 238 

9 10 9 

0.063 0.059 0.044 

0.010 0.022 0.026 

XXXII 

200 

12 

0.094 

0.027 

235 

20 

0.087 

0.019 

0.92 

0.91 

RRXLI 

236 237 238 

22 22 16 

0.575 0.145 0.111 

0.100 0.025 0.046 

so .... 0.008 0.035 0.078 0.010 0.012 0.046 0.029 0.07 0.008 0.010 0.022 0.026 O.ot8 0.098 0.024 0.045 

cv_ 32 28 19 53 17 9.2 37 84 35 16 37 59 21 17 16 41 

NAY 0.023 0.111 0.389 0.013 0.063 0.466 0.073 0.06 0.024 0.056 0.061 0.036 0.083 0.527 0.137 0.090 

NAU 0.008 0.035 0.083 0.010 0.013 0.049 0.030 0.07 0.008 0.010 0.022 0.026 0.019 0.100 0.025 0.046 

CV 35 32 21 77 20 11 41 110 35 18 36 73 23 19 18 51 

xCV 33 23 18 39 

(41_dmlNISTu1 

_______________ 

XLI: Sera 235-238
­

J13
 
Round Robin XU: Sera 235-238 Page I 

The attached N2M2QAP Round Robin XLI (RR41) Feedback includes: 

Pae "All Lab" Re ort 

1-4 A listing of all results for analytes reported by at least two laboratories, plus essential 

summary statistics 

5a A list of results for the four analytes reported by only one laboratory. 

5b A legend for the above two lists 

6 The "Measurement Comparability Summary" (or "Score Card") 

Pa e "Individualized" Re ort 

1 Your values, our assigned values, and the %bias between the two. 

2, 3 "Comparisons" plots for: retinol, retinyl palmitate, a- and y-tocopherol, total and 

trans-13-carotene, total a-carotene, total lycopene, 13-cryptoxanthin, lutein, and 

lutein & zeaxanthin. (There are insufficient zeaxanthin data to justify a separate 

plot, given that we need space for a Legend ... We do sum all individually reported 

lutein and zeaxanthin values into the "lutein & zeaxanthin" composite.) 

4 "Z-Score Concordance" plots for this RR's: retinol, a-tocopherol, y-tocopherol, total 

and trans-13-carotene, total a-carotene, and total and trans-1ycopene. 

5 %Bias Accuracy/Precision Summary of your last 3 years' results for: retinol, 

cx-tocopherol, y-tocopherol, total 13-carotene, and trans-13-carotene. 

6 NIST assigned value versus your value scatterplots of your last 3 years' results for: 

retinol, a-tocopherol, y-tocopherol, and/or total and trans-13-carotene. 

7-9 %Bias barchart of your last 3 years' results for: retinol, a- and y-tocopherol, and/or 

total and trans-13-carotene. 

Pae "SRM 968b" Re ort 

1, 2 "Comparisons" plots summarizing your RR32, RR34, RR39, RR40, and RR41 

results for the low-, mid-, and high-level components of SRM 968b with analytes: 

retinol, retinyl palmitate, ex- and y-tocopherol, total and trans-13-carotene, total acarotene, total lycopene, 13-cryptoxanthin, lutein, and lutein & zeaxanthin. (Again, 

there is insufficient zeaxanthin data to justify an individual analyte plot.) 

J14
 
 

Appendix K. “All-Lab Report” for RR41 

The following six pages are the “All-Lab Report” as provided to all participants, with two 

exceptions: 

• the participant identifiers (Lab) have been altered. 

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

The data summary in the “All-Lab Report” has been altered to ensure confidentiality of 

identification codes assigned to laboratories. 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. 

K1
 
Round Robin XLI Laboratory Results 

Values in μg/mL 

Retinol Retinyl Palmitate α-Tocopherol γ-Tocopherol δ-Tocopherol

Lab 235 236 237 238

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-BU 

FSV-BV 

FSV-BW 

FSV-BZ 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 

FSV-CH 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CX 

FSV-DA 

FSV-DB 

FSV-DJ 

FSV-DK 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DU 

FSV-EI 

FSV-EL 

FSV-EM 

FSV-FN 

0.307 0.657 0.956 !0.323 

0.283 0.620 0.889 !0.312 

0.266 

0.310 0.647 0.941 !0.232 

0.298 0.638 0.977 !0.303 

0.294 0.625 0.899 !0.319 

0.287 0.612 0.889 !0.304 

0.273 0.593 0.791 !0.322 

0.311 0.654 0.930 !0.325 

0.290 0.460 0.740 !0.23 

0.287 0.593 0.864 !0.3 

0.274 0.612 0.934 !0.307 

0.267 0.570 0.773 

0.276 0.578 0.825 !0.302 

0.324 0.711 0.966 !0.397 

0.280 0.610 0.890 !0.32 

0.364 0.589 0.859 !0.408 

0.351 0.587 0.851 !0.396 

0.283 0.540 0.857 

0.276 0.623 0.863 !0.303 

0.234 0.504 0.735 

0.250 0.560 0.790 !0.27 

0.294 0.646 0.931 

0.278 0.519 0.804 

0.283 0.635 0.841 !0.238 

0.275 !0.506 0.722 !0.289 

0.237 0.605 0.894 

0.248 0.544 0.760 !0.273 

0.248 0.589 0.861 

0.284 0.499 0.679 !0.249 

0.302 0.587 0.842 !0.282 

0.300 0.641 0.947 !0.331 

0.290 0.610 0.910 !0.26 

0.267 0.595 0.888 !0.29 

0.290 0.624 0.940 !0.322 

0.260 0.550 0.810 !0.28 

0.276 0.626 0.954 !0.326 

0.285 0.635 0.880 !0.31 

0.300 0.610 0.960 !0.29 

0.271 0.529 0.855 !0.26 

0.297 0.647 0.978 !0.318 

0.400 0.650 0.790 

0.268 0.580 0.807 !0.258 

0.291 0.599 0.977 !0.329 

0.258 0.553 0.811 

0.290 0.630 1.020 !0.3 

0.240 0.530 0.830 !0.23 

0.279 0.571 0.884 !0.315 

235 236 237 238 

0.082 0.30 0.092 !0.059 

0.056 0.26 0.064 !0.21 

0.075 0.36 0.118 !0.155 

0.109 0.16 0.116 !0.199 

0.118 0.20 0.082 !0.178 

0.089 0.34 0.091 !0.196 

0.063 0.14 0.044 !0.047 

0.109 0.20 0.093 

0.056 0.19 0.051 !0.04 

0.100 0.34 0.100 !0.1 

0.086 0.16 0.044 !0.035 

0.037 0.11 0.032 !0.054 

235 236 237 238 

7.07 11.44 19.3 !3.23 

7.05 13.18 22.2 !4.96 

7.17 

7.11 12.45 21.9 !2.06 

7.03 11.96 21.8 !3.71 

7.27 12.35 21.2 !5.9 

6.64 11.79 20.1 !4.42 

7.67 12.48 23.0 !6.21 

7.89 12.47 21.2 !5.03 

7.75 11.63 19.8 !5.6 

6.80 11.70 20.6 !3.8 

6.88 10.99 19.2 !4.42 

6.50 11.03 19.6 

6.76 11.85 19.8 

7.00 13.00 21.9 !5.5 

5.76 10.96 19.3 !3.7 

7.92 11.05 20.9 !5.76 

5.94 9.68 19.1 

6.80 11.00 19.6 !3.52 

6.60 11.80 21.2 !2.1 

5.63 8.79 16.1 

7.39 12.36 21.7 !4.55 

6.41 11.17 19.5 

7.34 11.90 19.9 

7.01 11.99 19.5 !2.84 

6.40 !7.2 20.0 !3 

5.48 9.03 15.3 

8.08 11.54 18.5 !5.21 

5.74 10.87 19.4 

12.19 15.83 21.6 !7 

7.20 10.90 20.7 <4.0 

7.11 12.12 20.8 !3.34 

7.62 12.31 20.9 !4 

6.80 11.30 20.4 !1.4 

6.40 10.43 17.3 !2.49 

6.91 11.52 20.7 !4.15 

5.98 10.98 20.4 !3.9 

7.19 11.84 20.0 !4.52 

6.50 11.80 20.7 !4 

7.40 11.35 19.6 !4.57 

6.57 11.81 17.4 

6.91 11.74 20.0 !4.55 

7.48 10.47 19.3 !5.34 

6.00 9.86 17.0 

7.16 11.01 19.0 !2.71 

6.37 10.50 19.4 !4.04 

235 236 237 238 

1.81 6.5 1.66 !1.42 

1.70 

1.70 6.2 1.12 !0.91 

1.72 6.5 1.29 !1.46 

1.49 5.6 1.10 !1.76 

1.59 6.3 1.12 !1.64 

2.34 8.7 0.38 !2.81 

1.79 6.9 1.35 !1.9 

1.46 5.9 0.98 !1.31 

2.19 5.3 1.83 !1.97 

1.75 6.4 1.23 

1.96 6.9 1.25 !1.73 

1.40 6.4 1.30 !0.95 

1.53 6.5 1.03 

1.83 6.0 1.29 

1.24 4.7 0.79 !1.21 

1.49 6.3 1.08 

2.13 6.3 0.79 !1.43 

1.58 5.9 0.93 !1.17 

1.62 6.1 1.19 !1.55 

1.41 5.9 1.15 !1.53 

2.00 6.9 1.19 !2.06 

1.32 6.3 0.54 

1.86 7.2 1.37 

1.60 5.8 1.18 !1.5 

235 236 237 238 

0.090 0.310 0.490 !1.04 

0.310 0.379 0.651 !0.98 

0.130 0.431 0.627 !0.93 

<0.3 0.400 0.600 !0.5 

0.090 0.170 0.550 !0.9 

0.076 0.371 0.540 !0.87 

n 48 46 47 38 12 12 12 11 46 44 45 34 25 24 24 18 5 6 6 6 

Min 0.234 0.460 0.679 0.230 0.037 0.11 0.032 0.04 5.48 8.79 15.3 1.4 1.24 4.7 0.38 0.91 0.076 0.170 0.490 0.50 

Median 0.283 0.602 0.864 0.303 0.084 0.20 0.086 0.10 6.96 11.58 20.0 4.1 1.70 6.3 1.16 1.52 0.090 0.375 0.575 0.92 

Max 0.400 0.711 1.020 0.408 0.118 0.36 0.118 0.21 12.19 15.83 23.0 7.0 2.34 8.7 1.83 2.81 0.310 0.431 0.651 1.04 

eSD 0.019 0.047 0.089 0.030 0.034 0.09 0.039 0.09 0.61 0.86 1.1 1.3 0.25 0.4 0.19 0.34 0.021 0.060 0.064 0.08 

eCV 7 8 10 10 41 45 45 89 9 7 5 31 15 7 17 23 23 16 11 9 

0.301 0.589 0.883 !0.224 7.56 12.24 20.9 !2.86 1.86 6.9 1.15 !1.17 nd 0.420 0.574 !0.6 

0.298 0.591 0.894 !0.242 6.97 11.27 20.3 !2.71 1.57 5.7 1.06 !1.05 0.091 0.326 0.529 !0.62 

0.291 0.596 0.876 0.268 0.084 0.20 0.086 0.10 7.11 11.67 20.3 3.4 1.71 6.3 1.13 1.31 0.091 0.374 0.563 0.76 

0.031 0.051 0.092 0.060 0.034 0.09 0.039 0.09 0.88 0.96 1.7 1.5 0.28 1.1 0.21 0.42 0.030 0.077 0.060 0.22 

NISTa
 

NISTb
 

NAV
 

NAU
 

All Lab Report K2 Page 1 / 6 
Round Robin XLI Laboratory Results 

Values in μg/mL 

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

Lab 235 236 237 238 235 236 237 238 235 236 237 238 235 236 237 238 

FSV-BA 0.255 0.301 0.35 !0.085 0.245 0.291 0.333 !0.082 0.010 0.010 0.016 !0.003 0.026 0.037 0.160 !0.01 

FSV-BD 0.261 0.303 0.44 !0.11
 

FSV-BE
 0.239
 

FSV-BF
 0.239 0.304 0.43 !0.036 0.027 0.034 0.325 !0.01 

FSV-BG 0.236 0.304 0.43 !0.074 0.021 0.028 0.219 !0.009 

FSV-BH 0.242 0.292 0.43 !0.105 0.229 0.277 0.407 !0.105 0.013 0.015 0.020 <0.01 0.015 0.024 0.266 !0.063 

FSV-BI 0.226 0.280 0.35 !0.077 0.018 0.020 0.184 !0.013 

FSV-BJ 0.229 0.268 0.31 !0.105 0.021 0.033 0.153 !0.027 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.243 0.280 0.46 !0.112 0.217 0.255 0.421 !0.092 0.015 0.015 0.025 !0.008 0.017 0.024 0.268 !0.011 

FSV-BO 0.212 0.255 0.30 0.021 0.027 0.180
 

FSV-BP
 0.470 0.488 0.69 !0.212 0.042 0.045 0.336 !0.036 

FSV-BQ 

FSV-BR 

FSV-BS >0.260 >0.290 0.260 0.290 !0.079 0.024 0.160 nq
 

FSV-BT
 0.262 0.267 0.38 !0.084 0.245 0.255 0.357 !0.079 0.017 0.012 0.019 !0.005 0.019 0.022 0.214 !0.026 

FSV-BU 0.270 0.333 0.45 !0.121 0.015 0.024 0.230 !0.02 

FSV-BV 0.251 0.294 0.40 0.014 0.021 0.202 

FSV-BW 0.278 0.365 0.46 !0.086 nq 0.017 0.223 nq
 

FSV-BZ
 >0.246 >0.290 >0.370 0.246 0.290 0.370 !0.08 0.010 0.009 0.009 nd 0.030 0.030 0.140 !0.02 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 0.145 0.274 0.28 0.011 0.016 0.161
 

FSV-CE
 0.220 0.260 0.49 !0.062 

FSV-CF 

FSV-CG 0.288 0.327 0.48 0.035 0.041 0.210 

FSV-CH 0.206 0.248 0.36 !0.078 0.009 0.013 0.192 !0.008 

FSV-CK 0.200 0.210 0.29 0.022 0.024 0.190
 

FSV-CL
 0.204 0.185 0.22 !0.052 0.021 0.028 0.152 !0.009 

FSV-CM 

FSV-CN >0.213 >0.259 >0.361 0.213 0.259 0.361 !0.051 nq nq 0.222 nq 

FSV-CQ 0.741 0.245 0.32 !0.012 

FSV-CR 

FSV-CS 0.277 0.290 0.41 !0.088 0.248 0.263 0.372 !0.08 0.029 0.027 0.035 0.028 0.030 0.268 !0.014 

FSV-CU 

FSV-CX 0.160 0.230 0.27 !0.02 0.010 0.010 0.120 !0.01 

FSV-DA 0.214 0.261 0.41 !0.066 0.189 0.233 0.380 !0.064 0.025 0.028 0.033 !0.002 0.019 0.038 0.217 !0.009 

FSV-DB 0.211 0.223 0.28 !0.076 

FSV-DJ 

FSV-DK 0.250 0.300 0.36 !0.085 0.019 0.027 0.196 !0.011 

FSV-DP 

FSV-DQ 0.290 0.320 0.29 0.021 0.022 0.096 

FSV-DR 0.213 0.251 0.26 !0.09 

FSV-DU >0.188 >0.282 >0.392 0.188 0.282 0.392 !0.122
 

FSV-EI
 >0.226 >0.252 >0.435 0.226 0.252 0.435 0.018 0.023 0.248 

FSV-EL 

FSV-EM 

FSV-FN 

n 29 28 28 22 10 11 11 10 7 7 7 6 24 26 27 17 

Min 0.145 0.185 0.22 0.012 0.188 0.233 0.290 0.051 0.010 0.009 0.009 0.002 0.009 0.010 0.096 0.008 

Median 0.239 0.280 0.37 0.085 0.228 0.260 0.372 0.080 0.015 0.015 0.020 0.004 0.020 0.024 0.202 0.011 

Max 0.741 0.488 0.69 0.212 0.248 0.291 0.435 0.122 0.029 0.028 0.035 0.008 0.042 0.045 0.336 0.063 

eSD 0.039 0.036 0.10 0.029 0.026 0.012 0.030 0.010 0.007 0.007 0.007 0.006 0.006 0.061 0.003 

eCV 16 13 27 34 11 5 8 13 49 49 37 30 25 30 27 

NISTa 

NISTb 

NAV
 

NAU
 

0.245 0.304 0.37 !0.051 0.214 0.205 0.298 !0.043 0.031 0.099 0.068 nd nd 0.160 nd 

0.237 0.261 0.37 !0.044 0.221 0.250 0.358 !0.044 0.017 0.011 0.011 0.027 0.037 0.210 !0.005 

0.240 0.282 0.37 0.066 0.222 0.243 0.350 0.062 0.019 0.036 0.030 0.023 0.030 0.194 0.008 

0.038 0.043 0.10 0.036 0.027 0.040 0.065 0.028 0.021 0.066 0.064 0.008 0.012 0.056 0.009 

All Lab Report K3 Page 2 / 6 
Round Robin XLI Laboratory Results 

Values in μg/mL 

Total Lycopene trans-Lycopene β-Cryptoxanthin α-Cryptoxanthin

Lab 235 236 237 238 235 236 237 238 235 236 237 238 235 236 237 238 

FSV-BA 0.110 0.33 0.152 !0.015 0.043 0.146 0.486 !0.017 

FSV-BD 0.140 0.38 0.18 !0.062 0.022 0.093 0.344 !0.02
 

FSV-BE
 

FSV-BF
 0.183 0.80 0.39 !0.036 0.019 0.116 0.438 !0.011 

FSV-BG 0.220 0.60 0.34 !0.071 0.100 0.47 0.222 !0.028 0.021 0.013 0.056 !0.018 

FSV-BH 0.198 0.82 0.35 !0.192 0.035 0.146 0.492 !0.05
 

FSV-BI
 0.138 0.33 0.17 !0.042 0.031 0.147 0.529 !0.024
 

FSV-BJ
 0.122 0.33 0.18 !0.065 

FSV-BK 

FSV-BL 

FSV-BM 

FSV-BN 0.183 0.86 0.38 !0.054 0.092 0.74 0.288 !0.041 0.031 0.154 0.600 !0.025 0.016 0.017 0.031 !0.007 

FSV-BO 0.273 0.61 0.31 0.027 0.122 0.395
 

FSV-BP
 0.305 0.86 0.42 !0.085 0.017 0.067 0.221 !0.007 

FSV-BQ 

FSV-BR 

FSV-BS 0.60 0.23 !0.07 0.150 0.460 !0.023
 

FSV-BT
 0.187 0.43 0.21 !0.061 0.148 0.39 0.180 !0.054 0.036 0.131 0.419 !0.033 0.020 0.015 0.014 !0.005 

FSV-BU 0.205 0.59 0.27 !0.042 0.031 0.150 0.463 !0.034 

FSV-BV 0.170 0.69 0.26 0.018 0.115 0.429 

FSV-BW 0.265 0.76 0.36 !0.054
 

FSV-BZ
 0.230 0.56 0.33 !0.14 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 0.117 0.28 0.14 0.023 0.103 0.257 

FSV-CE 

FSV-CF 

FSV-CG 0.146 0.46 0.23 0.029 0.125 0.417 

FSV-CH 0.083 0.34 0.17 !0.029 

FSV-CK 0.119 0.32 0.16 0.001 0.00 0.002 0.028 0.115 0.373 0.020 0.028 0.030
 

FSV-CL
 0.197 0.44 0.26 !0.06 0.020 0.099 0.269 !0.01 

FSV-CM 

FSV-CN 0.095 0.46 0.19 nq 0.019 0.136 0.478 !0.009 

FSV-CQ 

FSV-CR 

FSV-CS 0.184 0.36 0.22 !0.053 0.024 0.098 0.356 !0.017 

FSV-CU 

FSV-CX 0.120 0.45 0.12 !0.01 0.020 0.170 0.360 !0.01 

FSV-DA 0.191 0.81 0.43 !0.049 0.097 0.71 0.336 !0.029 0.024 0.079 0.398 !0.013 0.015 0.011 0.023 !0.005 

FSV-DB 0.198 0.42 0.22 !0.062 0.033 0.140 0.458 !0.023 

FSV-DJ 

FSV-DK 0.159 0.50 0.25 !0.033 

FSV-DP 

FSV-DQ 0.167 0.17 0.15 0.020 0.072 0.235 

FSV-DR 

FSV-DU 

FSV-EI 0.086 0.56 0.200 0.027 0.134 0.485 

FSV-EL 

FSV-EM 

FSV-FN 

n 26 27 27 20 7 7 7 5 23 24 24 17 4 4 4 3 

Min 0.083 0.17 0.12 0.010 0.001 0.00 0.002 0.015 0.017 0.013 0.056 0.007 0.015 0.011 0.014 0.005 

Median 0.183 0.46 0.23 0.057 0.097 0.47 0.200 0.029 0.024 0.124 0.418 0.018 0.018 0.016 0.027 0.005 

Max 0.305 0.86 0.43 0.192 0.148 0.74 0.336 0.054 0.043 0.170 0.600 0.050 0.020 0.028 0.031 0.007 

eSD 0.055 0.19 0.10 0.020 0.016 0.20 0.071 0.018 0.007 0.034 0.090 0.010 

eCV 30 42 42 35 17 43 36 61 31 27 22 58 

NISTa
 

NISTb
 

NAV
 

NAU
 

0.194 0.45 0.24 !0.018 0.087 0.34 0.156 !0.012 0.021 0.097 0.360 !0.007 

0.189 0.46 0.24 0.037 

0.048 0.21 0.11 0.033 

0.092 0.40 0.178 0.021 

0.022 0.22 0.073 0.015 

0.023 0.110 0.389 0.013 

0.008 0.040 0.095 0.012 

All Lab Report K4 Page 3 / 6 
Round Robin XLI Laboratory Results 

Values in μg/mL 

Lutein Zeaxanthin Lutein&Zeaxanthin Total Carotenoids 

Lab 235 236 237 238 

FSV-BA 

FSV-BD 0.070 0.47 0.064 !0.079 

FSV-BE 

FSV-BF 

FSV-BG 0.071 0.53 0.130 !0.081 

FSV-BH 0.054 0.46 0.069 !0.17 

FSV-BI 0.054 0.47 0.058 !0.064 

FSV-BJ
 

FSV-BK
 

FSV-BL
 

FSV-BM
 

FSV-BN
 0.062 0.54 0.076 !0.066 

FSV-BO 

FSV-BP 

FSV-BQ 

FSV-BR 

FSV-BS 

FSV-BT 0.088 0.44 0.107 !0.243 

FSV-BU 

FSV-BV 

FSV-BW 

FSV-BZ 0.080 0.97 0.120 !0.54 

FSV-CA 

FSV-CB 

FSV-CC 

FSV-CD 

FSV-CE 

FSV-CF 

FSV-CG 

FSV-CH 

FSV-CK 

FSV-CL 

FSV-CM 

FSV-CN 0.062 0.44 0.069 !0.063 

FSV-CQ 

FSV-CR 

FSV-CS 

FSV-CU 

FSV-CX 0.090 0.100 !0.08 

FSV-DA 0.046 0.53 0.075 !0.057 

FSV-DB 

FSV-DJ 

FSV-DK 0.076 0.50 0.114 !0.141 

FSV-DP 

FSV-DQ 

FSV-DR 

FSV-DU 

FSV-EI 0.069 0.55 0.082 

FSV-EL 

FSV-EM 

FSV-FN 

235 236 237 238 

0.023 0.051 0.055 !0.057 

0.015 0.063 0.024 !0.013 

<0.02 0.046 0.063 !0.31 

0.020 0.053 0.048 !0.044 

0.023 0.098 0.091 !0.063 

0.031 0.019 0.027 !0.022 

0.037 0.065 0.078 !0.05 

0.020 0.050 !0.02 

0.025 0.063 0.078 !0.044 

0.033 0.085 0.086 

235 

0.125 

0.093 

0.102 

0.086 

<0.07 

0.074 

0.074 

0.043 

0.119 

0.086 

0.090 

0.075 

0.091 

0.088 

0.080 

0.099 

0.077 

0.110 

0.071 

0.072 

0.072 

0.102 

236 

0.87 

0.52 

0.60 

0.59 

0.51 

0.52 

0.58 

0.37 

0.67 

0.46 

0.66 

0.58 

0.53 

0.63 

0.49 

0.38 

0.50 

0.46 

1.13 

0.59 

0.45 

0.62 

0.64 

237 

0.217 

0.119 

0.163 

0.154 

0.132 

0.106 

0.136 

0.063 

0.150 

0.134 

0.165 

0.155 

0.124 

0.175 

0.144 

0.086 

0.147 

0.129 

0.150 

0.153 

0.117 

0.072 

0.168 

238 

!0.235 

!0.136 

!0.08 

!0.094 

!0.48 

!0.108 

!0.106 

!0.19 

!0.265 

!0.136 

!0.072 

!0.113 

!0.15 

!0.1 

!0.101 

!0.08 

235 236 237 238 

0.70 1.44 1.40 !0.27 

n 

Min 

Median 

Max 

eSD 

eCV 

12 11 12 

0.046 0.44 0.058 

0.070 0.50 0.079 

0.090 0.97 0.130 

0.013 0.05 0.027 

19 10 34 

11 

0.057 

0.080 

0.540 

0.025 

32 

9 9 10 

0.015 0.019 0.024 

0.023 0.063 0.059 

0.037 0.098 0.091 

0.004 0.018 0.028 

19 28 48 

9 

0.013 

0.044 

0.310 

0.028 

64 

21 

0.043 

0.086 

0.125 

0.018 

21 

23 

0.37 

0.58 

1.13 

0.10 

18 

23 

0.063 

0.144 

0.217 

0.028 

20 

16 

0.072 

0.111 

0.480 

0.042 

38 

1 1 1 

0.70 1.44 1.40 

1 

0.27 

NISTa 

NISTb 0.056 0.43 0.067 !0.042 0.024 0.050 0.063 !0.028 0.080 0.48 0.129 0.59 1.30 1.35 !0.169 

NAV 

NAU 

0.063 0.47 0.073 

0.018 0.13 0.031 

0.061 

0.072 

0.024 0.056 0.061 

0.008 0.020 0.022 

0.036 

0.028 

0.083 

0.019 

0.53 

0.14 

0.136 

0.033 

0.090 

0.054 

All Lab Report K5 Page 4 / 6 
Round Robin XLI Laboratory Results 

Analytes Reported By One Laboratory 

Values in μg/mL 

Term 

n 

Min 

Median
 

Max
 

eSD 

eCV 

NAV 

NAU 

nd 

nq 

<x 

>x 

! 

italics 

Analyte Code 235 236 237 238 

Coenzyme Q10 FSV-CH 0.243 0.322 0.326 !0.109 

Total cis-β-Cryptoxanthin FSV-BT 0.012 0.007 0.008 !0.005 

trans-Anhydro-Lutein FSV-BT 0.040 0.046 0.041 !0.017 

trans-α-Carotene NISTb 0.019 0.024 0.197 !0.005 

Legend 

Definition

 Number of (non-NIST) quantitative values reported for this analyte

 Minimum (non-NIST) quantitative value reported

 Median (non-NIST) quantitative value reported

 Maximum (non-NIST) quantitative value reported

 Estimated standard deviation, calculated from the median absolute deviation

 from the median of the non-NIST results

 Coefficient of Variation for (non-NIST) results: 100*eSD/Median

 NIST Assigned Value, our estimate of the "true" analyte concentration

 NIST Assigned Uncertainty, our estimate of the total (serum hetergeniety and

 inter- and intra-laboratory) standard deviation

 For details on how we assign these quantities, see the "Analysis of Results."

 Not detected (i.e., no detectable peak for analyte)

 Detected but not quantitatively determined

 Concentration at or below the limit of quantification, x 

 Concentration greater than or equal to x

 Discrepant value: heterogeneous serum, damaged sample, malfunction, etc.

 Not explicitly reported but calculated by NIST from reported values

All Lab Report K6 Page 5 / 6 
Round Robin XLI Laboratory Results 

Lab R aT gT bC tbC 

FSV-BA 1 1 1 1 

FSV-BD 2 1 1 1 

FSV-BE 2 3 

FSV-BF 1 2 1 

FSV-BG 1 1 1 1 

FSV-BH 1 1 4 

FSV-BI 1 1 1 1 

FSV-BJ 2 1 3 1 2 

FSV-BK 1 1 1 1 1 

FSV-BL 2 2 1 2 

FSV-BM 1 2 2 

FSV-BN 1 

FSV-BO 3 1 

FSV-BP 1 2 4 1 

FSV-BQ 2 1 

FSV-BR 1 2 

FSV-BS 2 2 2 1 

FSV-BT 3 4 2 3

FSV-BU 1 1 1 3

FSV-BV 2 1

FSV-BW 1 1 4

FSV-BZ 1 1 2 1 2 

FSV-CA 2 2 2 2 

FSV-CB 1 

FSV-CC 2 1 1 

FSV-CD 3 2 1 1 1 

FSV-CE 1 

FSV-CF 3 2 

FSV-CG 1 1 

FSV-CH 2 3 1 2 

FSV-CK 1 1 

FSV-CL 1 1 

FSV-CM 2 1 1 3 

FSV-CN 2 1 2 1 

FSV-CQ 1 1 2 

FSV-CR 2 1 4 2 

FSV-CS 1 2 2 1 2 

FSV-CU 2 

FSV-CX 2 

FSV-DA 2 3 1 1 

FSV-DB 1 1 1 1 

FSV-DJ 1 1 

FSV-DK 1 1 1 2 

FSV-DP 2 1 

FSV-DQ 1 1 1 

FSV-DR 2 2 2 

FSV-DU 1 1 2 

FSV-EI 4 2 3 2 

FSV-EL 2 1 

FSV-EM 1 2 1 

FSV-FN 1 1 2 

NISTa 1 1 1 1 1 

NISTb 1 1 1 1 1 

n 48 46 25 29 11 

% Observed 

1 

Lab 

73 77 77 71 69 

2 22 17 12 23 31 

3 4 4 8 0 0

4 0 2 4 6 0 

All Lab Report 

Comparability Summary 

Definition

 laboratory number 

 "Standard Score" for Retinol 

 "Standard Score" for α-Tocopherol

 "Standard Score" for γ-Tocopherol

 "Standard Score" for Total β-Carotene

 "Standard Score" for trans-β-Carotene

number of (non-NIST) laboratories providing data for this analyte 

"Standard Score" 

Given that our knowledge of the shape, location, and width of the measurement distributions is 

approximate and that a limited number of labs are involved, we summarize comparability with the 

following four-level "Standard Score" (StS)... 

Label 

Lab

R 

aT 

gT 

bC 

tbC 

n 

StS 

1 

2 

3 

4 

where: 

StV 

NAV 

NAU 

t (1-α,n-1)

Expected 

68.2 % 

27.3 % 

 4.3 % 

0.3 % 

Definition

 All StV within ±t (1-0.683,n-1) {i.e., ±1 SD} 

 All StV within ±t (1-0.954,n-1) {i.e., ±2 SD} 

 All StV within ±t (1-0.997,n-1) {i.e., ±3 SD} 

 At least one StV > ±t (1-0.997,n-1) {i.e., >3 SD} 

 Standardized Value, the distance in standard deviation units your

 value is from the "true" concentration: StV = (your value - NAV) / NAU 

 NIST Assigned Value, our estimate of the "true" analyte concentration

 NIST Assigned Uncertainty, our estimate of the total measurement

 standard deviation (serum heterogeniety, analytical repeatibility,

 and among-laboratory reproducibility)

 Two-tailed Student's t for coverage of ±1, ±2, and ±3 NAU about

 NAV, assuming a normal population of size n 

These are the observed and normal-population-expected proportions of each Standard 

Score (StS), based upon each laboratory's largest StV for the four sera.

K7 Page 6 / 6 
 

 

 

 

 

Appendix L. Representative “Individualized Report” for RR41 

Each participant in RR41 received an “Individualized Report” reflecting their reported 

results. Each report included a detailed analysis of the results they reported for the 

following analytes: 

• Retinol 

• Retinol palmitate 

• α-Tocopherol 

• γ-Tocopherol 

• Total β-Carotene 

• trans-β-Carotene 

• Total α-Carotene 

• Total Lycopene 

• trans-Lycopene 

• β-Cryptoxanthin 

• Lutein 

• Lutein & Zeaxanthin 

In addition, each participant in RR41 received an “SRM 968b Report” that summarized 

their results for the three components of SRM 968b in RR32, RR34, RR39, RR40, as 

well as in RR41. This summary addressed all of the above analytes except transLycopene. 

The software systems used to generate the original “Individualized Report” and the 

“SRM 968b Report” are no longer available and we do not have hardcopy of the report 

sent to participant FSV-BA. We do, however, have hardcopy for a NIST analyst; pages 

L2 to L10 are the “Individualized Report” and pages L11 and L12 are the “SRM 968b 

Report” provided to analyst NISTb. 

Pages L13 to L22 were produced for the results of participant FSV-BA using a 

descendant of the 1997 software. Although the form of the presentation has changed 

radically, three of the graphical tools used in the original reports (“Boxplot 

Comparisons”, “Z-Score Concordance”, and “NIST Assigned Values Vs Laboratory 

Values”) have been retained and display the same information in much the same manner 

as in the original. The current software does not provide the “% RSD Bias and Precision 

History” table nor the “% Difference” plots. 

L1
474 

Individualized Round Robin XLI Report: NISTb 

Your Data, NIST Assigned Values, and %Differences 

Serum235 Serum 236 Serum237 

Analyte You NAV %A n You NAV %A n 11 You 

Retinol 0.298 0.291 2 46 0.591 0.596 -1 46 0.894 

a-Tocopherol 6.97 7.09 -2 44 11.3 11.6 -3 44 20.3 

y-Tocopherol 1.57 1.71 -8 23 5.67 6.28 -10 23 1.06 

~-Tocopherol 0.091 0.091 1 5 0.326 0.374 -13 6 0.529 

Total p-Carotene 0.237 0.242 -2 27 0.261 0.281 -7 27 0.369 

trans-p-Carotene 0.221 0.222 -1 10 0.250 0.244 2 11 0.358 

Total a-Carotene 0.027 0.024 12 23 0.037 0.030 21 25 0.210 

trans-a-Carotene 0.019 0.024 0.197 

Total Lycopene 0.194 0.189 3 25 0.453 0.467 -3 26 0.240 

trans-Lycopene 0.087 0.092 -6 7 0.342 0.404 -15 7 0.156 

P-Cryptoxanthin 0.021 0.023 -9 22 0.097 0.111 -13 23 0.360 

Total Carotenoids 0.586 1 1.30 1 1.35 

"Lutein&z.eaxanthin" 0.080 0.083 -5 20 0.479 0.527 -9 22 0.129 

"Lutein" 0.056 0.063 -11 12 0.429 0.466 -8 11 0.067 

"Z-eaxanthin" 0.024 0.024 2 9 0.050 0.056 -12 9 0.063 

You : Your reported values for the listed analytes (micrograms/milliliter) 

NAY : NIST Assigned Values, equal to (NISTs average-of-averages+ this Round Robin's median)/ 2 

%.:\ : Percent difference between your value and the NA V 

* : Non-quantitative value: heterogeneous serum, damaged sample, procedural error, etc. 

Please check our recorded values against your records. 

NAV %A n II 

0.880 2 46 *

20.3 0 44 *

1.14 -7 23 *

0.563 -6 6 *

0.372 -1 27 *

0.350 2 11 *

0.196 7 26 *

*0

0.242 -1 26 *0

0.178 -12 7 *0

0.389 -8 23 *0

1 *0

0.137 -6 22 *0

0.073 -8 12 *0

0.061 3 10 *0

Send corrections to: N2M2QAP 22218208, NIST, Gaithersburg, MD 20899; fax 301-977-0685; email David.Duewer@NIST.gov 

L2
47S 

10f30/97 

-E!l@~-

I 

200 200 23S 236 

200 2C17 235 

I 

236 

Individualized Round Robin XLI Report: NIST

Boxplot Comparisons 

I 

237 

I 

237 

I 

238 

-

I 

238 

200 200 23S 

l 

0 

8 

~ -I!]- -I!]--~ -

200 200 235 

Ei3 

I 

236 

I 

236 

I 

237 

I 

237 

8 

238 

B 

I 

238 

200 2C17 23S 

200 200 23S 

L3
476 

~ 

8. 

200 207 23!5 

0 rei • 

~-~--EI -(j-

~ 

200 '1J.Y1 23!5 

10f30/97 

• 

I 

236 

I 

236 

Individualized Round Robin XLI Report: NIST

Boxplot Comparisons (Continued) .------~~~~~

I 

237 

I 

237 

238 

238 

-~--~--~-

200 '1J.Y1 23!5 

200 207 23!5 

B 

• 

236 

I 

236 

I 

237 

I 

237 

-

,__ 

.... 

I 

238 

I 

238 

200 '1J.Y1 23S 

Solid circles: Your d

Box plots: Top - 7

Bottom 

Middle 

Width - 

200,207,235: Low-le

236: New se

237: New se

238: New, p

L4
477 

Individualized Round Robin XLI Report: NISTb 

Z-Score Concordance 

3 

Retinol --TC=I 

-------TC=2 

+ Others 

() NIST 

a-Tocopherol y-Tocopherol 

• You 

2 ------ + -- . + 

+,-- + ·._ -+: 

' 

- 

t' 

' >. 1 

g 

~ 

:+ + 

+ : 

* -+/* Cl) 

·-

§ 0 

u 

j Total & trans-fl-Carotene Total a-Carotene Total & trans-Ly

0 

§ 3 

u 

+ 

. 

.+ 

. 

+ '+ 

+ ' . + +\ 

' 

' 

' . ' + + 

' ++ 

¥i*

+ + + 

-3 -2 -1 0 2· 3 -3 -2 -1 0 2 3 -3 -2 -1 

__ .,.. Average Concordance-<111-- __ .,.. Average Concordance ... --- __ .,.. Average 

l<Vl!W7 

L5
478 

RR 

XXXII 

XXXIII 

XXXIV 

xxxv 

XXXVI 

XXXVII 

xxxvm 

XXXIX 

XL 

XLI 

lonot97 

Individualized Round Robin XLI Report: NISTb 

%RSD Bias and Precision History 

P-Carotene 

Retinol a-Tocopherol y-Tocopherol Total 

~ vA ~ vA l1lfi vA mA vA 

0 1 0 0 1 1 2 1 

4 3 -8 2 -2 5 -28 16 

1 3 -1 0 2 2 3 

-3 4 -7 6 -11 4 -3 

1 1 3 1 2 3 -2 

-3 3 1 4 2 4 -6 

-4 3 1 3 5 2 1 

-4 3 -6 4 -9 3 -16 

0 1 -1 2 -1 3 

1 2 -2 2 -8 1 

%A was traditionally evaluated %A Evaluation 

0-5% Exceptional 

6-10% Acceptable 

11-20% Marginal 

>20% Poor 

0 

-3 

However, there is no single set of criteria that is appropriate 

for all analytes, at all levels, for all purposes. 

1 

4 

3 

6 

7 

9 

4 

3 

trans 

l1lfi 

3 

-26 

-1 

-4 

0 

-3 

4 

-10 

-4 

1 

vA 

0 

13 

3 

4 

3 

6 

6 

7 

5 

2 

Interpretation 

Precision and bias are separate aspects of meas

Precision can be estimated as vA, the standard 

bias as mA, the average %A, for all (valid) sera 

%A Percent relative difference from Nist As

%A = 1 OO(Your value - NA V) I NA V 

NA V NIST Assigned Value, our best estimate 

NA V = (NISTs average-of-averages + R

l1lfi Mean difference, the average %A for all 

vA Difference variability, one standard devi

It's best to be unbiased and precise (small mA, 

Good precision (small vA) with bias (large lllfi) 

such values are internally consistent and may b

once the relative biases are known. 

Poor precision (large vA) suggests that your me

adequate control for the analyte levels examine

L6
479 

1000/97 

- ±1 eSD 

--· ±3 eSD 

, , , 

. , , , , 

, , 

, 

. 

, 

. , 

, , 

, , 

, 

, 

, 

Individualized Round Robin XLI Report: NISTb 

NIST Assigned Values Vs Laboratory NIST3 Values 

Retinol 

, 

, 

, , , 

, 

, 

. 

, 

, , 

, , , 

. , 

, , 

, , , 

, , 

, 

, , , 

, 

, 

. , 

, 

, 

, 

, 

, 

, , 

, 

, 

, 

, 

, 

, 

- ±1 eSD 

--· ±3 eSD 

A Total 

0 trans 

P-Carotene 

, 

, 

, 

, , 

, 

, 

, 

, 

, 

, 

, 

, 

Leg

Open Symbols: 

Black Symb

Abscissa (X-axis): N

Ordinate (Y-axis): Y

Interpr

, , 

, 

, 

, 

If much of your data is 

±3 eSD lines, your mea

inadequately precise. 

, 

, 

, 

a-Tocopherol 

- ±1 eSD 

--· ±3 eSD 

, 

. . , , 

. ,' 

, , , , 

. , 

. 

. , 

, 

. 

, 

. 

, 

, 

, , 

, 

y-Tocopherol 

- ±1 eSD 

--· ±3 eSD 

. . ____ , 

, . . . . , 

, 

, 

• 

• 

• I 

. , 

, , 

, 

. , , 

, 

, 

• , . 

, 

, 

, 

, 

, 

, , 

, 

, 

, 

, , , 

, , 

, 

, , 

, 

, 

. , , 

If your data are system

the NIST Assigned Val

system is biased relativ

of N2M2QAP participan

If there are one or two 

may be calculation or tr

Please check your subm

the original data. 

The "eSD" calculations 

Duewer, et al . Analytic

69(7): 1406-1413. 

L7
480 

> 

< 

~ ...-.. 

> 

~ 

~ 

d 

* 0 

0 

-

<I 

~ 

IOIJ0/97 

50 

25 

0 

-25 

-50 

x 

x 

x 

I 

I 

I 2 2 2 

9 0 0 0 

9 0 I 2 

Individualized Round Robin XLI Report: NISTb 

Retinol, %.!\ in Round Robin XXXII - XLI 

x 

x 

x 

I 

I 

I 

2 2 2 2 

0 0 0 0 

3 4 5 6 

2 2 2 2 

0 0 0 I 

7· 8 9 0 

2 2 2 2 

I I I I 

I 2 3 4 

2 2 2 2 

I I I I 

5 6 7 8 

x 

x 

x 

v 

I 

I 

2 2 2 2 

I 2 2 2 

9 0 I 2 

Serum 

x 

x 

x 

v 

I 

I 

I 

2 2 2 2 

2 2 2 2 

3 4 5 6 

2 2 2 2 

2 2 2 3 

7 8 9 0 

L8
481 

50 

25 

> 

< x ~ x ...-.. 

> x 

< I z I 

~ 0 

d 

* 

0 

0 

-

<1 

~ 

-25 

-50 

I 2 2 2 

9 0 0 0 

9 0 I 2 

IOl30l97 

Individualized Round Robin XLI Report: NISTb 

Tocopherols, %~ in Round Robin XXXII - XLI 

x 

x x x 

x x x x 

x x x v 

I X V I 

I I 

Iltpi ~,- ~~) ~ bl • X• ~~'.:,~ ~ 

:·,.·. .···· 

X 

L 

• g-Tocopherol El a-Tocopherol 

2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 

0 0 0 0 0 0 0 I I I I I I I I I I 2 2 2 2 2 2 2 2 2 2 3 

3 4 5 6 7· 8 9 0 I 2 3 4 5 6 7 8 9 0 I 2 3 4 5 6 7 8 9 0 

Serum 

L9
482 

50 

25 

> 

< x ~ x "'""" 

> x 

< I z I 

.g 0 

d 

* 0 

0 

.-4 

<] 

~ 

-25 

-50 

I 2 2 2 

9 0 0 0 

9 0 I 2 

IO/Jll/CJ7 

Individualized Round Robin XLI Report: NISTb 

B-Carotenes, %L\ in Round Robin XXXII - XLI 

x 

x x x 

x x x x 

x x x v 

I x v I 

I v I I 

I I 

Iyr . ' ,. 

• trans-8-Carotene Im Total 8-Carotene 

2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 

0 0 0 0 0 0 0 I I I I I I I I I I 2 2 2 2 2 2 2 2 2 2 3 

3 4 5 6 7. 8 9 0 I 2 3 4 5 6 7 8 9 0 I 2 3 4 5 6 7 8 9 0 

Serum 

L10
123 

g 

~ 

0 

«i 

.... 

·5 

I I I 

200 1U1 235 

-a_ K _ ----- ll.c-

~ - - -~- - •;j 

~ 

I I I 

200 1U1 23S 

IOl'.!AJ/'J7 

I I I I 

201 209 234 

I 

I I I I 

201 209 234 

SRM 968b Report: Laboratory NISTb 

-e 

! 

~ _I!)~ 

j 

~ 

~ 

I I I I 

I I I I I I I I I I I I I 

I I I I I I I 

202 210 227 200 1U1 23S 201 209 234 202 210 227 200 1U1 23S 201 

I - _O_ - - - - I I I 

l!I B 

• •• 0 

- c: 

e £ 

.8 ~-~~ ~ g. u 

~ 

I 

co. I 

VI 

~s-~-~ ~ 

-8--~- -i.- - - - - - - ----- --

I I I I I 

I I ~ 2;,, ~s I ~I ~ ~ I I I I 

I I I I I I 

202 210 227 202 210 227 200 1U1 23S 201 

L11
124 

SRM 968b Report: Laboratory NISTb 

-.-- -- - -- -

• 

-·--·--·-- ---Q 

UH 

.W.::lH: 

~s= 

·~ - - -- --·--

~ 

200 '}ff/ 23S 201 209 234 202 210 m 200 '}ff/ 23S 201 209 234 202 210 227 200 '}ff/ 23S 201 

~ ~ ~ ~ 

Solid circles: Your dat

- -

- Box plots: Top - 75

v Bottom - 

s= lil 

8. 

rn 1 

Middle - 

0 Width - P

C,) 

s 

"; Light lines: Solid - C

0 u ~ I Dotted - 

cc. 

200,207,235: SRM 96

201,209,234: SRM 96

200 '}ff/ 23S 201 209 234 202 210 227 200 200 23S 201 209 234 202 210 227 202,210,227: SRM 96

10/30/97 

L12
 Set 1 of 52 

Individualized Round Robin XLI Report: FSV-BA 

Summary 

Analyte 

Retinol 

α-Tocopherol 

γ-Tocopherol 

Total β-Carotene 

trans-β-Carotene 

Total cis-β-Carotene 

Total α-Carotene 

trans-Lycopene 

β-Cryptoxanthin 

Lutein&Zeaxanthin 

Serum 235 

You NAV 

0.307 0.291 

7.07 7.11 

1.81 1.71 

0.255 0.240 

0.245 0.222 

0.010 0.019 

0.026 0.023 

0.110 0.092 

0.043 0.023 

0.125 0.083 

n 

48 

46 

25 

29 

10 

7 

24 

7 

23 

21 

Serum 236 

You NAV 

0.657 0.596 

11.4 11.7 

6.45 6.28 

0.301 0.282 

0.291 0.243 

0.010 0.036 

0.037 0.030 

0.332 0.404 

0.146 0.110 

0.874 0.527 

n 

46 

44 

24 

28 

11 

7 

26 

7 

24 

23 

Serum 237 

You NAV 

0.956 0.876 

19.3 20.3 

1.66 1.13 

0.349 0.368 

0.333 0.350 

0.016 0.030 

0.160 0.194 

0.152 0.178 

0.486 0.389 

0.217 0.136 

n 

47 

45 

24 

28 

11 

7 

27 

7 

24 

23 

Serum 238 

You NAV 

!0.323 0.268 

!3.23 3.44 

!1.42 1.31 

!0.085 0.066 

!0.082 0.062 

!0.003 

!0.01 0.008 

!0.015 0.021 

!0.017 0.013 

!0.235 0.090 

n 

38 

34 

18 

22 

10 

6 

17 

5 

17 

16 

You : Your reported values for the listed analytes (micrograms/milliliter)
 

NAV : NIST Assigned Values, here equal to this RR's median
 

n : Number of non-NIST laboratories reporting quantitative values for this analyte in this serum 

Please check our records against your records. Send corrections and/or updates to... 

Micronutrients Measurement Quality Assurance Program 

National Institute of Standards and Technology Tel: (301) 975-3935 

100 Bureau Drive Stop 8392 Fax: (301) 977-0685 

Gaithersburg, MD 20899-8392 USA Email: david.duewer@nist.gov 

Individualized Report Page 1 / 10 

L13
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

Retinol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 2 / 10 

L14
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

α-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 3 / 10 

L15
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

γ-Tocopherol, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 4 / 10 

L16
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

Total β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 5 / 10 

L17
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

trans-β-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 6 / 10 

L18
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

Total α-Carotene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 7 / 10 

L19
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

trans-Lycopene, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 8 / 10 

L20
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

Total β-Cryptoxanthin, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 9 / 10 

L21
 

 

 Set 1 of 52 

Individualized RR XLI Report: FSV-BA 

Total Lutein&Zeaxanthin, μg/mL 

[Analyte], μg/mL 

Your [Analyte], μg/mL 

Median [Analyte], μg/mL 

200207235236

237238 

Apparent Precision, SD 

Concordance, SD 

3rd Quartile (75%) You, this RR You, ≥x, this RR NIST, this RR 

Median (50%) You, past RRs You, ≥x, past RRs Others, this RR 

1st Quartile (25%) Expectation You, poor sample 

The software that was used to produce the original "Individualized Reports" for this study is no longer available. The original reports provided 

the same graphical analyses but in different format. This sheet was generated using a descendent of the 1997 system. For details of the 

construction and interpretation of these plots, see: Duewer et al. Anal Chem 1999;71(9):1870-8. 

Serum Comments History 

#235 Lyophilized, multi-donor, native. This is the Low level of SRM 968b. RR32 #201, RR34 #209 

Lyophilized, prepared from a "low" single donor pool augmented with many #236 New anayltes to ≈10% of normal population level.
 

Lyophilized, prepared from a "low" single donor pool augmented with many
 #237 New anayltes to ≈50% of normal population level. 

Lyophilized, prepared from a "low" single donor pool augmented with many
 

#238 anayltes to ≈90% of normal population level. This material is heterogeneous; New
 

results for this material are not used to access performance.
 

Individualized Report Page 10 / 10 

L22
 

 

Appendix M. Shipping Package Inserts for RR10 

The following two items were included in each package shipped to a RR10 participant: 

•	 Cover letter and instructions for preparing the Control Sample 

•	 Report of Analysis datasheets for the preparation of the Control Sample and for 

the analysis of the Control and Serum Samples 

The cover letter and datasheets were enclosed in a sealed waterproof bag along with the 

samples themselves. 

M1
Dr. Margolis printed a separate cover letter for each 

participant. The "FIELD( )" statements are commands 

for a mail-merge macro routine. 

M2
M3
M4
M5
 

Appendix N. Final Report for RR10 

The following 11 pages are the final report as provided to all participants. This report 

contains: 

•	 Cover letter and analysis of results 

•	 Table 1 “Results of Round Robin RR10 for the Measurement of AA in Human 

Serum” 

•	 Table 2 “Results of Round Robin RR10 for the Measurement of AA using NIST 

AA Sample” 

•	 Legend for the following four Figures 

•	 Figure 1 “Tukey Box Plot of the Round Robin RR09 Results” 

•	 Figure 2 “Tukey Box Plot of the Round Robin RR10 Results” 

•	 Figure 3 “Distribution of Round Robin RR10 Results for lots 682a and 682b” 

•	 Figure 4 “Distribution of Round Robin RR10 Calculated and Measured Results 

for the Ascorbic Acid Standard” 

A number of the results reported in Tables 1 and 2 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
 
November 4, 1997 

FELil(Title) :f11BLDfFirst) ~))~ast) 

FIBL!'(Company) 

FleL!l(Address) 

Dear FlfiLJl(Title:) D(Las* 

This report describes both the overall-group and your laboratory performance in Round Robin X 

for the measurement of ascorbic acid (AA) in human plasma. This study involved the duplicate 

analyses of two unknown samples, 682a and 682b and a solid ascorbic acid sample as a 

standard. Your results are designated as Lab. No. - in the tables and figures. 

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

data were not included in the statistical analysis). Two laboratories submitted two sets of 

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

Standard Deviation (%RSD) for both lots was 15.1 and 14.5. The intralaboratory %RSD varied 

from 0.4-5.1 with one exception. 

These results indicate that the intralaboratory variation remains essentially unchanged from the 

two previous round robins (0.3-4.0). However, the interlaboratory %RSD is similar to that of RR 

IX (13.9 and 11.8) and has increased slightly. The box plots in Figures 1 and 2 graphically 

summarize the results, the highest and lowest 10% of the measurements for each lot are plotted 

as small open circles, the two simple lines each span the next 15% intervals, and the center box 

contains the values from the remaining data sets. The NIST mean value for the total ascorbic 

acid + dehydroascorbic acid is represented by a solid circle. The horizontal line in the 50% 

boxes represents the median interlaboratory values which are nearly identical to those of NIST 

serum ascorbic acid concentrations. 

In RR IX we asked each laboratory to make up a solution from solid ascorbic acid, measure its 

UV absorbance, and assay the ascorbic acid content. Unfortunately, the concentration was low 

except for several laboratories who increased the concentration 10 fold. The purpose of this 

segment of the study was to try to evaluate the role that your standards and your measurement 

technique might be playing in the accuracy and precision of your measurement process. In RR X 

we asked you to perform the same measurements on ascorbic acid solutions that were ten times 

more concentrated. These results are summarized in Table 2. The ascorbic acid concentrations 

were calculated from the weights that you reported, and the volume of metaphosphoric acid 

(MP A) was calculated by using a density of 1.004 g/L for 5% MP A. The analysis of the weights 

of a 500 μL aliquot of the AA stock solution gave a mean of 513 mg, SD 10.2, %RSD 2.0 (range 

490-527 mg). The analysis of the results of the conversion of the weighed amount of 100 mL of 

MP A in to the 100 mL volumetric flask was a mean of 102.5 g, SD 0.96, %RSD 0.94 (range 99-

103 g). These data indicate that the laboratories are able to accurately weigh samples between 

0.500 and 100 g. It also indicates that the pipettes used to measure sub mL volumes is biased 

Dr. Margolis printed a separate letter for each 

participant. The "FIELD( )" statements are 

commands for a mail-merge macro routine. 

N2
 
high by 2.5% at 500 μL. An important question that is not answered in this study is whether this 

is a constant bias or proportional to the volume being measured. However, it strongly suggests 

that each laboratory should calibrate its micropipettes over the range that they are used. One way 

to do this is to weigh a series of aliquots (5-10) of a liquid such as water, convert the weights to 

volumes using the density of water, and calculate the accuracy and precision of the pipette and 

pipetting technique. Using the data that you submitted to us, we calculated the concentration of 

the AA in the standard solution (column 1, Table 2) which each of you made and assumed that 

the error in concentration was no greater than the error in weighing 0.5 to 100 g. The amount of 

AA that you actually measured in your assay of the standard solution is listed in column 2, Table 

2. To compare the measurements on the standard solutions, we normalized all of the data 

obtained by assaying the standard solution to a starting concentration of 50 μmol/L using the 

equation: 

assayed [AA l = normalized [AA l 

weighed [AA} 50 

The results of this calculation are summarized in column 3, Table 2. The mean of these data is 

49.1, SD 4.9, %RSD 10.1(range39.3 - 54 μmol/L). If the estimated error in weighing and in 

filling the volumetric flasks is small (1 - 2%), then the major source of error is in the assay itself. 

This would include the accuracy of the pipets, the accuracy of the standards particularly if they 

are diluted, the accuracy of the volume of the sample standard and/or serum) delivered to the 

assay mixture, and the accuracy of any constants used in the calculation of the concentration of 

the analyte from the results of the assay. These calculations exclude the data from laboratory 1 

which made up its stock solution 1/10 that of the desired value, laboratory 13 which made an 

additional 1 :20 dilution of its diluted stock solution and laboratory 30 whose data concerning the 

standard solution we could not interpret. Finally we asked each of you to measure the 

absorbance of your standard solution at 243 and 244 nm. Every laboratory obtained similar 

values at each wave length indicating that the wavelength was correct; however, the mean E1% for 

a 1 cm cell was 555 AU/mole/cm, SD 25, %RSD 4.5. At NIST the E1% was determined for 

Fisher and Sigma samples of AA and the values were 529 and 533 AU/mole/cm respectively. 

The reported values varied from 501to606 AU/mole/cm excluding laboratory 1 which made up 

its stock solution 1/10 of the desired value and laboratory 30 whose data concerning the standard 

solution we could not interpret. These results without the excluded data indicate that there is a 

need among some laboratories to calibrate their spectrophotometers with absorbance standards 

such as SRM 2031. 

In conclusion we can identify the following sources of systematic bias in the measurements. 

1. The spectroscopic error in the measurement of the absorbance of a standard solution 

(%RSD = 4.5) 

2. The pipetting of aqueous solutions mean 2.5% above expected value 

3. The weighing of samples 0.5-100 g (%RSD of 1and2% respectively) 

4. The measurement of the concentration of a 50 μmol/L standard solution (mean= 49.1 

μmol/L, %RSD = 10.1). The mean value is close to the expected value therefore the 

error probably lies in the accuracy of the measurement of the sample or the 

calculation constants. 

5. The measurement of the serum AA (%RSD = 14.5 and 15.1). This could either reflect 

N3
 
an error in delivering the total sample to the assay because of the viscosity of the 

sample or in the constants used in calculating the AA concentration. 

If your values differed from those of NIST by more than 5%, we suggest that you evaluate 

whether you accurately deliver the correct sample volume that can vary either as a function of the 

sample viscosity or the accuracy of the pipet. Alternatively, we suggest that you evaluate the 

accuracy of the constants that you use in converting the assay results to a final AA concentration 

in the serum. If your results deviate significantly from the assigned values, we would suggest 

that you reexamine your methods for possible systematic errors. The distribution of the results 

of each laboratory are graphically illustrated in Figures 3-7. 

The next set of samples (RR XI) will be shipped during November, 1997. If you have any 

questions concerning the previous round robins please contact me at 301/975-3137 or by e-mail 

at sam.margolis@nist.gov. 

Sincerely, 

Sam A. Margolis, Ph.D. 

Research Chemist 

Analytical Chemistry Division 

Chemical Science and Technology Laboratory 

Enclosures 

N4
 
Table 1 Results of Round Robin X for the Measurement of AA in Human Serum 

Ascorbic Acid (μmol/L Serum)a 

Lot 682b Lot 682a 

106.0 ± 2.0 74.5 ± 1.5 

119.5 ± 3.9 85.9 ± 1.3 

125.0 ± 0.0 89.5 ± 0.6 

113.8 ± 4.3 71.0 ± 5.1 

105.4 ± 0.7 82.2 ± 1.8 

140.6 ± 0.4 100.3 ± 2.1 

90.8 ± 0.6 66.1 ± 3.2 

110.8 ± 1.3 79.0 ± 0.3 c 86.4 ± 0.7 

91.7 ± 1.4 63.9 ± 2.0 

124.6 ± 2.3 89.1 ± 2.3 

121.4 ± 0.7 85.2 ± 0.5 

87.6 ± 0.6 63.4 ± 0.6 

112.2 ± 10.5 84.3 ± 4.2 

136.8 ± 2.4 92.8 ± 1.5 

94.5 ± 0.1 72.5 ± 2.0 

139.6 ± 1.0 101.1±1.1 

120.7 ± 1.1 85.9 ± 5.1 

108.0 ± 2.9 80.2 ± 1.2 

112.5 80.9 

17.0 11.7 

15.1 14.5 

115.4 ± 2.7d 83.2 ± 5.5d 

100.1 ± l.6d 70.7 ± l.8d 

a Values represent the mean and SD of replicate measurements on two samples (total of 4 

measurements). 

b The abbreviations in this column are as folows: LC, liquid chromatography; DNPH, 

dinitrophenylhydrazine; EC, electrochemical detector; ENZ, enzymatic assay; DCIP, 

dichloroindophenol; AUTOAN, autoanalyzer; OPD, orthophenlyenediamine. 

N5
 
c The wrong sample was sent and therefore the results are not included. 

d Values represent the mean and SD of replicate measurements on five samples (total of 10 

measurements). 

N6
 
Table 2 Results of Round Robin X for the Measurement of AA using NIST AA Sample 

Lab Method Ascorbic Acid (μmol/L MPA) E1%a 

Calculated Measured Normalizedb 

LC 5.81 5.80 49.9 790 

DNPH 

LC-EC 

ENZ 59.2 62.8 53.0 552 

DNPH 

DCIP 51.1 46.3 45.2 533 

DCIP 55.6 55.1 49.1 569 

LC-EC 56.9 61.5 54.0 553 

LC-EC 57.9 62.6 54.0 561 

LC 

LC-EC 29.0 26.2 45.2 555 

LC 29.4 28.7 48.9 606 

LC-EC 

59.7 46.9 39.3 556 

AUTO AN 59.2 57.5 48.5 546 

LC-OPD 57.7 59.6 51.7 556 

LC-EC 54.0 43.7 40.4 603 

LC-OPD 56.2 59.2 52.6 576 

LC 58.2 61.8 53.2 541 

LC-EC 

56.5 45.4 40.2 528 

DNPH 35.9 35.7 49.7 501 

ENZ 63.5 68.4 53 .9 544 

LC 55.9 

Mean 49.1 555c 

SD 4.9 26 

%RSD 10.1 4.7 

NIST Sigma (5% MPA) 533 

NIST Fisher (5% MPA)d 529 

Lit. (aqueous solution) 560 

a Absorptivity of a 1 % solution in a 1 cm cell. 

b The standard values for each laboratory were dependent on the amount of AA weighed by 

each lab. In order to compare the measured AA concentrations of each laboratory, the 

measured values were normalized to correspond to a weighed value of 50 mmol/L. 

c This value does not include the results of laboratory 1. 

d This sample was obtained from the Center for Disease Control. 

N7
 
Figure 1. Tukey Box Plot of the Round Robin X Results. 

The open circles represent the highest and lowest 10% of the measurements. The two simple 

lines each span the next 15% intervals and the center box contains the values from the remaining 

data sets. The NIST mean value for the total ascorbic acid (AA+ DRAA) is represented by a 

solid circle. The horizontal line in the 50% box represents the median inter-laboratory values 

which are slightly different from the NIST values. 

Figure 2. Tukey Box Plot of the Round Robin X Results. 

The open circles represent the highest and lowest 10% of the measurements. The two simple 

lines each span the next 15% intervals and the center box contains the values from the remaining 

data sets. The NIST mean value for the total ascorbic acid (AA+ DRAA) is represented by a 

solid circle. The horizontal line in the 50% box represents the median inter-laboratory values 

which are slightly different from the NIST values. 

Figure 3. Distribution of Round Robin X Results for lots 682a and 682b. 

0 First Vial; First Measurement 

o First Vial; Second Measurement 

t:.. Second Vial; First Measurement 

o Second Vial; Second Measurement 

The solid points 3:1"e for Lot 682a 

The open points are for Lot 682b 

Figure 4. Distribution of Round Robin X Calculated and Measured Results for The Ascorbic 

Acid Standard. 

The open squares represent the measured AA concentration. 

The solid diamonds represent the calculated AA concentration. 

N8
 
Round Robin IX 

0 

80 

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-0 

E 60 

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-

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< 

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20 0 

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688a 188a 

Lot Number. 

N9
 
140 

120 

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(.) 

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L... 8 60 

en 

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Round Robin X 

1 

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Lot Number. 

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AA Std. 

N10
 
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Distribution of RR X Results for Lots 682 a and b. 

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a-------. ---- - --- -- ----- - . -·-- ·----·-·---- . ----- --- ------------- )- -·--- 

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10 15 20 25 30 

Laboratory No. 

N11
Distribution of RR X Results on the AA Standard 

80 ~~~~~.,--~~~~~~~~~r--~~~~r--~~~--,r

70 t- --------t 

~ 60 I t o ? : --r------ -- J- • 8 ~ 

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Laboratory No. 

20 

N12
 

Appendix O. “All-Lab Report” for VC-RR10 

The following is a single page “All-Lab Report” that 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 for the Serum Samples have been corrected and transformed to have units 

of μmol/mL sample. 

•	 results for the Control and Serum Samples have been consolidated. 

•	 additional summary statistics have been included. 

O1
Vitamin C Round Robin 10 

Control Solution Ascorbic Acid, mmol/mL 

O2

AA, μmol/mL Ratio 682B 682A 

E1% 

Obs/Cal Lab Method Cal Obs Sdup dL/gcm Mean Sdup Srep Shet Stot Mean Sdup Srep Shet 

VC-MA HPLC-EC 565 54.3 2.3 0.0 ­ 58.2 1.0 0.2 1.0 1.0 40.5 0.3 0.1 0.3 

VC-MB AO-OPD 564 58.5 62.8 0.4 1.07 61.5 0.0 0.0 0.0 0.0 44.8 0.0 0.4 0.0 

VC-MC HPLC-EC 802 5.8 5.8 0.2 1.01 53.0 0.0 1.2 0.0 1.2 37.2 0.3 0.9 0.0 

VC-MD 24DNPH 59.8 0.5 2.3 0.0 2.3 42.9 0.7 0.4 0.6 

VC-ME HPLC-UV 565 57.1 57.5 1.4 1.01 62.3 1.0 1.0 0.7 1.2 44.6 0.9 0.9 0.6 

VC-MF HPLC-EC 552 58.6 59.6 0.8 1.02 60.7 0.1 0.4 0.0 0.4 42.6 0.2 0.2 0.1 

VC-MG HPLC-EC 594 54.9 61.8 0.4 1.13 68.4 0.3 1.5 0.0 1.5 46.4 0.5 0.7 0.0 

VC-ML 24DNPH 562 59.1 46.9 0.9 0.79 45.9 0.2 0.8 0.0 0.8 32.0 1.1 0.5 1.1 

VC-MO HPLC-EC 55.9 0.2 54.0 1.3 1.2 1.0 1.5 40.1 0.7 0.2 0.7 

VC-MQ HPLC-UV 578 55.0 55.1 1.3 1.00 52.7 0.0 0.4 0.0 0.4 41.1 1.1 0.2 1.1 

VC-MS AutoAnal 533 55.9 45.4 1.1 0.81 47.2 0.0 0.1 0.0 0.1 36.2 1.0 0.7 0.9 

VC-MV HPLC-OPD 560 56.3 61.5 0.6 1.09 70.5 0.3 0.3 0.2 0.4 50.1 1.2 0.4 1.2 

VC-MW 24DNPH 507 35.5 35.7 0.2 1.00 69.8 0.4 0.4 0.3 0.5 50.6 0.3 0.6 0.0 

VC-MX HPLC-EC 611 29.2 28.7 0.2 0.99 43.2 0.4 0.2 0.3 

VC-MZ HPLC-EC 560 28.7 26.2 0.1 0.91 55.4 0.6 0.5 0.5 0.7 39.5 0.0 0.2 0.0 

VC-NB HPLC-UV 609 53.4 43.7 0.2 0.82 43.8 0.2 0.3 0.0 0.3 31.7 0.0 0.4 0.0 

VC-ND HPLC-EC 583 55.6 59.2 0.5 1.06 56.1 6.1 1.9 6.0 6.3 42.5 1.4 2.5 0.0 

VC-NG HPLC-EC 566 57.2 62.6 1.09 45.4 0.1 0.3 0.0 0.3 33.0 1.7 1.1 1.5 

VC-NJ AO 551 62.8 68.4 1.2 1.09 60.3 0.6 0.3 0.6 0.6 42.9 0.9 3.0 0.0 

VC-NO HPLC-UV 538 50.6 46.3 4.6 0.91 56.9 2.3 0.9 2.2 2.4 35.5 1.8 2.6 0.0 

N 18 18 19 20 19 20 

Mean 578 49.4 46.6 0.99 56.9 40.9 

SD 61 15 19 0.10 8 5 

CV 11 30 41 11 14 13 

Min 507 5.8 2.3 0.0 0.79 43.8 0.0 0.0 0.0 0.0 31.7 0.0 0.1 0.0 

Median 564 55.3 55.1 0.5 1.00 56.9 0.3 0.4 0.0 0.7 41.8 0.7 0.5 0.2 

Max 802 62.8 68.4 4.6 1.13 70.5 6.1 2.3 6.0 6.3 50.6 1.8 3.0 1.5 

eSD 20 4 12 0.10 6 4 

eCV 4 7 22 10 11 10 

All Lab Report