eo enevisr 2 Feoby Fro sy National Jhstitute of Stindards & Technology Sa Certificate of Analusis Standard Reference Material” 17f Sucrose Optical Rotation “This Standard Reference Material (SRM) is intended primarily for use as a saccharimetry standard in calibrating lanes systema, "The certified chemical purty and reference values forthe optical rotation of a “rormal rarer” (described below) of SRM 17f Sucrose at 20.00 °C # 0.01 °C in a 10000 mm cell and a 200,00 men cell prided, A unit of SRM I7Fconsiss of one bottle containing 60 g of erystalline sucrose Certified Purity and Uncertainty: A NIST certified value is a value for which NIST has the highest confidence in its accuracy in that all known or suspected sources of bias have been investigated or taken into account (1). The certified chemical purity of sucrose was determined by measuring the mass fractions of impurities including water, ther saceharides, and residue from ashing, summing the impurities, and subtracting this sum from 100 %, Certified Purity of Sucrose as a Mass Fraction: 99.956 % + 0.004 % ‘The uncertainty in the certified value is expressed as an expanded uncertainty, U, at the 95 % level of confidence, and is calculated according to the method described in the ISO Guide (2]. The expanded uncertainty is calculated as U = hug, where us intended to represent, atthe level of one standard deviation, the uncertainty in the measurement of the impurities. The coverage factor, k= 2, is determined from the Student's f-distribution corresponding to the appropriate degrees of freedom and approximately 95 % confidence. Reference Values and Uncertainties: Reference values are noncertified values that represent a best estimate of the true value; however, the values do not meet the NIST criteria for certification and are provided with associated uncertainties that may reflect only measurement precision, may not include all sources of uncertainty, oF may reflect ' lack of sufficient statistical agreement among multiple methods [I]. Reference values for the optical rotation of 2 “normal sugar solution” of SRM 17f at four wavelengths are provided in Table 2a in both milliradians and degrees (Gee “Preparation of a Normal Sugar Solution”). Table 2b includes the reference value for the °Z value for a “normal sugar solution” of SRM I7f. The unit, °Z, is the unit of the “Intemational Sugar Scale” defined by the International Commission for Uniform Methods of Sugar Analysis (ICUMSA). The reference value for the specific rotation is provided in Table 2c. Expiration of Certification: The certification of SRM 17f is valid, within the measurement uncertainties specified, until 01 July 2023, provided the SRM is handled and stored in accordance with the instructions given in this certificate (see “Notice and Warnings to Users”). The certification is nullified if the SRM is damaged, contaminated, or otherwise modified. NIST will monitor this SRM over the period of its certification. If substantive technical changes occur that affect the certification before expiration, NIST will notify the purchaser. Registration (see attached sheet) will facilitate notification, ‘The overall direction and coordination of technical activities leading to certification of this SRM were under the leadership of K.W. Phinney of the NIST Biomolecular Measurement Division. Carlos A. Gonzalez, Chief Chemical Sciences Division Gaithersburg, MD 20899 Robert L, Watters, Jr., Director Certificate Issue Date: 29 March 2013 Office of Reference Materials Cerificate Revision History on Last Page SRM 17 Page 1 of 4enonta, LT. Sniegoski, ana by DM en ramet MA omelet Meneame cp BK MT nese omen asurement Cpemical Sc#EnEES als Deviston: natal me wea arihe NIST & 2 tu ARN ne tem Coane sy Not Zhngorihe nist sansa “nee antes tous the NIST OME 1 analyses were proved! Stans ce of this SKM were 600% ween approximately 20°C peratures between Pe must be eB ‘drying prior 10 use, TE «bin its oniginal bottle at tery Material will not fequsre re and hieht AND WARNING TO USERS ‘The SRM should be store Storage and handling. ths (ed from excessive moist Storage and U and 25°C, With proper Aercapped after usage and protec s Hawaiian Sugar Company SOURCE, PREPARATION, AND ANAL: wided by the California and “The material used for this SRM was Pro ror very accurate reasurerents,sausion offs SRE peut prepared ents gar scion” 3s efi si ‘onder ster cited water. “nora fog fealy reared wns sose weighed in vacuum disolved in pa water, 7 sie 100.009 auataey 2601606 of ae ra surne et 100000¢ Les SIT pe pepe Ta eae ee wate 1 a tal as of 10000 g. Adon WIC pepo of SRO 17 and adr Se ond in ference 3 In pace, on cn amuse) Py oun at ees smal ua ee pty the eberved ovation bythe ratio of 23,7018 ote acta mass 1° ommpare resets wit the reference values in Table 23 fom Analyses: Analyses for value assignment of the optical rotation of SRM formed at JASCO, Ine. (Easton, MD). nat solution of SRM 17, provided in Table 2, is based on the Intemations! SUs=t Fr 0022 point ofthe Intemational Sugar Scale corresponds to the se atthe wavelength of $46.2271 nm in @ 200.000 mm Source of Material: (Crockett, CA). Preparation of a Normal Sugar Solution: le conditions using pul 17f provided in Optical Rotatic Table 2a were pe ‘The optical rotation of a nor ‘Scale, which became effective July 1, 1988 optical rotation caused by a normal solution of pure sucro polariscope tube at 20.00 °C (3}- lemental analysis results of SRM 17f and the theoretical percentages ‘Additional Analyses: Table 1 provides the el secilated for CrsHO1y. Thus, the comparison shows that the theoretical composition 18 well within the incertainty of the elemental analysis measurements ‘Table 1. Theoretical Composition and Elemental Analysis of CyaH::0u, for SRM 17f SRM 17fResults Theoretical Calculation Element (%) (%) c 4222 4 0.12 2.10 H 647 + 0.10 648 are expressed as expanded uncertainties, U, atthe 95 % level of confidence, and ee WHETE axe ealoulated according to the method described in the ISO Guide [2]. The expanded uncertainty is calculated as U up's intended to represent, at the level of one standard deviation, the effects of between-lab variati ‘The co fi . ; ab variation. ‘The coverage faster, 1 mene ee ing e aproie dee of Hc 3d appro 95 % confidence. © The uncertainties in the elemental analysis results Karl Fischer titration yielded a moisture content of aj / .pproximately 0.097 mg/g. Results of nuclear magnetic resonance (NMR) analysis were consistent with a purity > 99 %, and additional supporting analyses indicated that there was no significant contribution from other saccharides. wa es Cant commercial eaipmentisirumeniation, or materials a identified in this certificate to adequately specify th expel prose, Suc aiiaon ds ot ingly recommendation or endorsement by NIST, nor does it imply that or equipment identified are necesserily the best available for the purpose. Page 2 of 4 SRM 17fICUMSA Equation: Using the rotatory dispersion equation below, given by ICUMSA (4), values for the optical rotation at 632.9914 nm and XX2 60 nm were calculated {rom the measured values at $46,271 nm. ‘These values are shown in Table 2a. “This equation was also used to calculate a value for the optical rotation at $49.4400 nm. ‘This value agreed to within 0.2 % of the average measured rotation for this SIM at 549.4460 nm, a Fava aos My ta-A' 4a, y= -0075 087 659 000 a, 43,588 221 904 58S az = 0.051 946 178 300 a, = -0:006 $15 194377 a ‘wavelength (jm) Table 2a. Reference Values" forthe Optical Rotationofa “Normal Sugar Solution” of SRM I7fata Temperature of 20.00 °C * 0.01 °C Wavelength 100.00 mm Cell Optical Rotation 200.00 mm Cell Optical Rotation (vacuo, non) (evrad) (degrees) (mrad) (degrees) $4622 35568 £ 071 20379 + 0041 T1136 #142 40.758 + 0.082 589.4400" 30203 + 060 17.305 + 0035 604.06 + 121 34.610 + 0.069 © 62.9914" 25951 £052 14.869 + 01030 519.02 £ 104 29.737 + 0.060 882.60 12941 + 026 ©7414 + OOS 25881 + 052 14829 = 0.030 Table 2b. Reference Value” for ° at $46.2271 nm of a “Normal Sugar Solution” of SRM 17f at 20.00 °C + 0.01 °C °Z = 99.953 + 0.201 Table 2e, Reference Value for the Specific Rotation (a]” of SRM 1 at $89.4400 am Specific Rotation, [a]: 66.517 + 0.134 The uncertainties inthe reference values are ex in the reference values are expressed as expanded uncertainties, U, atthe 95% {lela according tothe method described inthe ISO Guide 2]. The expanded uncertainty is calelated as Ulan, where t, tended represen athe eve of oe standard deviation, the combined elect of wihinatned senavon we tees amceinty component, The eoverge factor ks determined om ine Stents o Rem degrees Pica and approximately 95 % confidence. ae aoe il roton values for 594400 wn, 6329946 am ott te SO ibm 2904. HNO nm we Gea bt go Be meses ‘The uncertainty for the ° value also inludes a component for uncertainty in the 100 level of contidence, and are °Z value (3), SRM 17f Page 3 of 4REEERENCES (1) May, We Paris, Ri eck H.C asset J; Greenberg, Ra Guenther, Bi Kramer, Gs Wise, S. Gills, Ts Colert Js Gettings, Ri; MacDonald Ij Definition af forms and Moses Used at MIST for Value Assignment of Reference Materials for Chemical Measurements, NIST Special Publication 200-136 (206%), available at IntpAnW nist gow/smMVpload/SI'260-16 PDF (nccessed March 201%). [2], 106M 100-2008; Evaluation of Measurement Data — Guide to the Expression of Uncertainty in Measurement (GUM 1995 with Minor Comrections); Joint Committee for Guides im Metrology (2064), available. at Jp twa. bipm org/utils/common/documentscm/ICGM. 100 2008 F pdf (accessed March 2013), see also Taylor, BLN Kuyatt, CE; Guidelines for Evaluating and Expressing the Uncertainty of HIST Measurement Results; NIST Technical Note 1297; U.S. Government Printing OMfice: Washington, DC (19/4); available at bttp:/www.nist.gov/pml-pubs/in]297/index.efm (accessed March 2013), [8] ICUMSA ~ Methods Book, Method GS2/3-1; The Braunschweig Method for the Polarization of White Sugar by Polarimenry, \CUMSA Publication Department: Norwich Research Park NR4 7UB, England (1944), [4] ICUMSA Proceedings 1998, 22nd Session; Bartens: Berlin, Germany; p. 209 (199%) Certificate Revislon History: 29 March 2019 (Extension of corfieation period, edtoral changes, 09 Jane 2010 (This revision cludes aa Updated certified value for purty, updated uncertainties for the elemental analysis, updated reference values for opicl rotation, and minor editorial changes.) 26 May 2009 (Editorial revisions): 8 August 2008 (Original ceria issue dat), Users of this SRM should ensure that the Certificate of Analysis in their possession is current. This can be ‘accomplished by contacting the SRM Program: telephone (301) 975-2200; fax (301) 948-3730; e-mail srminfo@nist gov; or via the Internet at http:/Avww.nist.govisri. SRM 17f Page 4 of 4 >