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YBB60122012: Tests for Release of Arsenic Antimony Lead and Cadmium
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.