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YBB 60122012: PDF in English

YBB 60122012 YBB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA Tests for Release of Arsenic Antimony Lead and Cadmium Tests for Release of Arsenic Antimony Lead and Cadmium This method is applicable to the determination of the release of arsenic antimony lead and cadmium in various types of medicinal glass containers and pipes. Preparation of test product solution When the test product is a container, the sampling quantity is shown in the table below: When the test product is a glass tube, take a glass tube with a total surface area (including the inner and outer surfaces of each tube and the cross-sections at both ends) of approximately 500 cm2, and finely grind the cross-sections at both ends as the test product. Preparation of test product solution: Clean the test sample. Fill to 90% of full capacity with 4% (v/v) acetic acid solution. For containers with smaller capacity such as ampoules, fill the acetic acid solution to the neck of the bottle. Cover the mouth with an inverted beaker (made of borosilicate glass with an average linear thermal expansion coefficient a (20~300°C) of approximately 3.3×10-6K-1; new beakers must be aged) or aluminum foil of inert material. Steam at 98°C for 2 hours. After cooling, take out the test sample. The solution shall be the test solution. Clean the glass tube for testing. Place into a glass container filled with 1000ml of 4% (v/v) acetic acid solution (the glass container shall not contain arsenic, antimony, lead, and cadmium elements). Steam at 98°C for 2 hours. After cooling, take out the test sample. The solution shall be the test solution. 1 Determination of release of arsenic Test principle The high-valent arsenic contained in the test solution is reduced to trivalent arsenic by potassium iodide and stannous chloride. Then it reacts with zinc particles and acid to produce new ecological hydrogen and generate arsine. After being absorbed by the silver salt solution, a red colloidal substance is formed. Compare with the standard curve or specified limits to determine its content or control its limits. Method One: Determination by standard curve Accurately measure 10 ml of the test solution, 10 ml of the blank solution, and 1 ml, 2 ml, 3 ml, 4 ml, and 5 ml of the standard arsenic solution (each 1 ml is equivalent to 1 μg of As) (the linear range can be adjusted according to the actual situation of the sample if necessary). Respectively place them in arsenic testing bottles. Measure according to the law (Chinese Pharmacopoeia Edition 2010, Part II, Appendix VIII J, Method Two). Measure the absorbance at a wavelength of 510 nm. Draw a standard curve with concentration as the X-axis and absorbance as the Y- axis. Determine the concentration of the test solution by comparing it with the standard curve. Method Two: Determination by limit checking Precisely measure 10 ml of the test solution, 10 ml of the blank solution, 2 ml of the standard arsenic solution (each 1 ml is equivalent to 1 μg of As) (when measuring the container), 3.5 ml (when measuring the pipe). Respectively place them in arsenic testing bottles. Measure according to the law (Chinese Pharmacopoeia Edition 2010, Part II, Appendix VIII J, Method Two). Respectively measure the absorbance at a wavelength of 510 nm. The absorbance of the test solution shall not be higher than that of the standard arsenic solution. Results representation For glass containers, the result is express as As (mg/l). For glass pipes, it is expressed as As (mg/dm2). 2 Determination of release of antimony Test principle Malachite green (C23H25N2Cl) forms a green complex with pentavalent aluminum ions. It is extracted with toluene. The organic phase is extracted for colorimetry. Compare to a standard curve or to specified limits. Determine its content or control its limits. Method One: Determination by standard curve Precisely measure 10 ml of test solution, 10 ml of blank solution, and 0.5 ml, 1 ml, 1.5 ml, 2 ml, 2.5 ml of standard antimony solution (each 1 ml is equivalent to 1 μg of Sb) (the linear range can be adjusted according to the actual situation of the sample if necessary). Respectively place in separating funnels. Add 10 ml of hydrochloric acid (1→2) to each. Add 6 drops of 10% stannous chloride-hydrochloric acid solution to each. Shake well. Place for 1 minute. Add 1 ml of 14% sodium nitrite solution (newly prepared for temporary use) to each. Shake well. Add 1ml of 50% urea solution to each. Shake until bubbles disappear. Add 1 ml of phosphoric acid (1→2), 10 ml of water, 10 ml of toluene, 0.5 ml of 0.2% malachite green solution respectively. Shake for 1~2 minutes. After leaving to separate, discard the water layer. Take the toluene layer. According to UV-visible spectrophotometry (Chinese Pharmacopoeia Edition 2010, Part II, Appendix IV A), measure the absorbance at a wavelength of 634 nm. Draw a standard curve with concentration as the X-axis and absorbance as the Y-axis. Determine the concentration of the test solution by comparing it with the standard curve. ......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.