CAFFEINE MELTING POINT STANDARD CERTIFIED REFERENCE MATERIAL

Transcription

1 CAFFEIE MELTIG POIT STADARD CERTIFIED REFERECE MATERIAL O CH 3 H 3 C O CH 3 LOT #: BCBD3894V Fluka o OMIAL WT: 1 g CERTIFICATE VALIDITY DATE: 12. October 2010 VERSIO: BCBD3894V-1 ote: Certificates may be updated due to Compendial Lot changes or the availability of new data. Check our website at: for the most current version. EXPIRATIO: SEP / 2013 (Proper Storage and Handling Required) STORAGE: Store at Room Temperature/Protect from Light, keep container tightly closed. Attachment of a 20 mm aluminum crimp seal recommended for unused portions. CHEMICAL FORMULA: C 8 H 10 4 O 2 MW: PHYSICAL DESCRIPTIO: White powder in amber vial CAS #: HAZARDS: Read MSDS before using. Always handle as if potentially hazardous using prudent laboratory techniques. ISTRUCTIOS FOR USE: Dry over silica gel for 16 hours prior to use. The internal pressure of the container may be slightly different from the atmospheric pressure at the user s location. Open slowly and carefully to avoid dispersion of the material. This material is intended for LABORATORY USE OLY and OT for use in humans or animals. Certificate of Analysis Version BCBD3894V-1 Page 1 of 5

2 CERTIFIED MELTIG RAGE/POIT Specification: The observed range falls within the acceptance range: 1.0 range between and C (USP) DETERMIATIO METHOD: All samples were dried for 16 hours over silica gel prior to use. The melting range/melting point of the Caffeine Melting Point Standard was determined concomitantly with the melting range/melting point of the USP Caffeine Melting Point Standard using the capillary method. This method provides traceability to the USP Reference Standard. Instrument: Mettler Toledo FP900 Thermosystem with FP81 Measuring Cell Temperature Program: C to C at 0.2 C/min MELTIG RAGE Expanded Uncertainty LOT: BCBD3894V C C ± 0.10 C, k = 2 USP LOT: K0D C C ± 0.10 C, k = 2 MELTIG POIT LOT: BCBD3894V C ± 0.10 C, k = 2 USP LOT: K0D C ± 0.10 C, k = 2 Temperature Program: C to C at 1.0 C/min MELTIG RAGE Expanded Uncertainty LOT: BCBD3894V C C ± 0.12 C, k = 2 USP LOT: K0D C C ± 0.13 C, k = 2 MELTIG POIT LOT: BCBD3894V C ± 0.12 C, k = 2 USP LOT: K0D C ± 0.12 C, k = 2 Certificate of Analysis Version BCBD3894V-1 Page 2 of 5

3 ote: The expanded uncertainty values for the USP Reference Standard do not contain a component of homogeneity, since this information is not available from the USP. LOSS O DRYIG/VOLATILES (VOL) Specification: Specified for USP Caffeine Melting Point Standard Method: Dry over silica gel for 16 hours Mean of three samples, Loss = 0.02% IDETIFICATIO TESTS IFRARED SPECTROPHOTOMETRY FTIR COMPARISO OF CAFFEIE MELTIG POIT STADARDS Fluka o. RTP01653 %T USP cm-1 RTP Fluka Caffeine Melting Point Standard Lot: P BCBD3894V USP Caffeine Melting Point Standard Lot: K0D372 PERKI ELMER SPECTRUM 100 SAMPLIG: UIVERSAL ATR Certificate of Analysis Version BCBD3894V-1 Page 3 of 5

4 1 H MR (Data provided by an external laboratory) Consistent with Structure ELEMETAL AALYSIS (Data provided by an external laboratory) Specification: ot more than 0.3% difference between theoretical and experimental Exeter Analytical 440 Elemental Analyzer Combustion method Results of duplicate analysis: % Theoretical Experimental Mean C H HOMOGEEITY ASSESSMET Between-bottle homogeneity was assessed in accordance with ISO Guide 35. Completed units were sampled over the course of the bottling operation. Samples were taken in the following manner: the units produced in the bottling operation were divided into three chronological groups, those from the Early third, the Middle third, and the Late third (Groups). A pre-determined number of sample units were then randomly selected from each group. A subset of each group was then randomly selected for chemical analysis. The results of the chemical analysis were then compared by Single Factor Analysis of Variance (AOVA). Certificate of Analysis Version BCBD3894V-1 Page 4 of 5

5 AALYTICAL METHOD: MELTIG POIT An analytical sample was prepared from each of four bottles from each Group (Early, Middle, and Late/twelve total). Sample size: ~ 3.2 mg Replicate (triplicate) analysis was performed on each sample. The order of replicate analyses was randomized. The between bottle standard deviation was derived from the AOVA. o significant difference between the Groups was indicated. Heterogeneity was not detected under the conditions of the AOVA. Certified by Reviewed by Validity Date Quality Systems THIS PRODUCT WAS DESIGED, PRODUCED AD VERIFIED BY RTC- USA FOR ACCURACY AD STABILITY I ACCORDACE WITH ISO 17025:2005 (ACLASS Cert AT-1467) and ISO GUIDE 34:2009 (ACLASS Cert AR-1470). Certificate of Analysis Version BCBD3894V-1 Page 5 of 5