独立行政法人　産業技術総合研究所

[This document is just explanation translated from the original Japanese certificate and some information is omitted from it.] National Institute of Advanced Industrial Science and Technology This certified reference material (CRM) was produced based on quality system in compliance with JIS Q 0034 (ISO GUIDE 34), for use in calibration of analytical instruments, quality control of analytical instruments, and validation of analytical techniques and instruments.
Certified Value
The certified value is purity (in mass fraction), given in the following table. The expanded uncertainty was determined using coverage factor k = 2, corresponding to an estimated confidence interval of approximately 95 %. Analytical Methods
The certified value is the weighted mean of purities (in mass fraction) determined by subtraction method and nuclear magnetic resonance (NMR) method. In the subtraction method, impurities were analyzed using high performance liquid chromatograph with ultra violet detector (HPLC/UV), high performance liquid chromatograph with corona charged aerosol detector (HPLC/CAD), Karl-Fischer titration, head space – gas chromatograph / mass spectrometer (HS-GC/MS) and thermogravimeter (TG). In the NMR analysis, 1,4-bis(trimethylsilyl)benzene-d4 was used as the internal standard. The combined standard uncertainty was estimated by the combination of standard uncertainties due to purity determinations by subtraction method and by NMR, difference between the methods and homogeneity. Traceability
Organic impurities were determined with HPLC/UV, HPLC/CAD and HS-GC/MS by using standard solution prepared by gravimetric blending method by NMIJ. Water content was determined by Karl-Fischer titration, which is one of the primary methods of measurements. Ignition residue was determined with TG calibrated with weight. Mass fraction of 17β-estradiol was determined with NMR by using 1,4-bis(trimethylsilyl)benzene whose purity was assayed with a differential scanning calorimeter and NMR, as an internal standard. The certified value is traceable to the SI. Expiration of Certification
The expiration date of the certification for this CRM is March 31st, 2017 under the condition of storage, indicated in “Precautions Sample Form
The form of this CRM is white powder at ambient temperature. 300 mg was sealed in an amber glass vial with argon gas. The glass vial is sealed into an aluminum-laminated bag. Homogeneity
[This document is just explanation translated from the original Japanese certificate and some information is omitted from it.] The homogeneity was measured by analysing ten vials selected from 400 vials by stratified random sampling method in order of subdivision. Total concentrations of non-volatile organic impurities, water and ethanol were determined by HPLC/UV, KF and HS-GC/MS, respectively. From the results, variation of purity (in mass fraction) between and within the vial(s) was estimated as homogeneity. This is reflected in the uncertainty of the certified value. Instructions for Storage
This CRM should be stored in a cold (around 5 °C) and dark place. Store the CRM according to its material safety data sheet Instructions for Use
This CRM is for laboratory use only. This CRM should be stored to reach at ambient temperature before opening. This CRM is hygroscopic and should be used as soon as possible after opening. From the homogeneity, a minimum sample mass of 20 mg should be used for each measurement or sample preparation. Instructions for Handling
Wear protective equipments such as safety glasses, safety mask and safety gloves in handling. Handle the CRM according to the Preparation of CRM
This CRM was purified and subdivided by Wako Pure Chemical Industries, Ltd. This CRM was prepared by purifying a commercial high purity reagent. 300 mg of purified 17β-estradiol is filled into the amber glass vial in argon atmosphere. Information
Concentrations of 1,3,5,6,8-estrapenten-3,17β-estradiol, 6-dehydro-17β-estradiol, 17α-estradiol, 1-methyl-17β-estradiol, estrone, 4-methyl-17β-estradiol, 3-methyl-17β-estradiol, water and ethanol are 0.28 g/kg, 0.08 g/kg, 0.13 g/kg, 0.34 g/kg, 1.13 g/kg, 4.9 g/kg, 0.04 g/kg, 7.5 g/kg and 0.07 g/kg, respectively. Water, ethanol and other impurities were determined with KF, HS-GC/MS NMIJ Analysts
Technical manager for this CRM is K. Kato. The production manager is Y. Shimizu. The analysts are Y. Shimizu, T. Saito, Y. Technical Information
Customers will be notified in the case of important revision, such as a change in the certified value. Technical information about this CRM can be obtained from the contact shown below. Reproduction of Certificate
In reproducing this certificate, it should be clearly indicated that the document is a copy. National Institute of Advanced Industrial Science and Technology If you have any questions about this CRM, please contact National Institute of Advanced Industrial Science and Technology, [This document is just explanation translated from the original Japanese certificate and some information is omitted from it.] Metrology Management Center, Reference Materials Office, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563, Japan Tel: +81-29-861-4059; Fax: +81-29-861-4009, http://www.nmij.jp/ Note: This certificate is a translation of the original Japanese certificate and is not an official document.

Source: https://www.nmij.jp/english/service/C/crm/42/6004a_en.pdf