This standard specifies the physical, mechanical, marking and packaging requirements for radiopaque and radiolucent cured polymeric resin bone cements, primarily based on polymethacrylates. YY 0459-2003 Surgical Implants Acrylic Resin Bone Cement YY0459-2003 Standard download decompression password: www.bzxz.net

YY 0459-2003/ISO 5833:2002
This standard is equivalent to ISO5833:2002 "Surgical implants - acrylic resin bone cement" (English version). This standard is equivalent to the translation of ISO5833:2002. For ease of use, this standard has made the following editorial changes: a) "this international standard" is changed to "this standard", b) the decimal point "," is used instead of the comma ","", c) the foreword of the international standard is deleted.
Appendix A, Appendix B, Appendix C, Appendix D, Appendix E, Appendix F of this standard are normative appendices. This standard is proposed by the State Food and Drug Administration. This standard is under the jurisdiction of the National Technical Committee for Standardization of Surgical Implants and Orthopedic Devices. This standard was drafted by Tianjin Institute of Synthetic Materials Industry. The main drafters of this standard are: Dou Hongyi, Xu Shiqing, Wang Fengxia, Wang Shufang, Lin Huanwen. I
1 Scope
YY0459--2003/IS05833:2002
Acrylic resin bone cement for surgical implants This standard specifies the physical, mechanical, marking and packaging requirements for radiopaque and radiolucent cured polymeric resin bone cements, mainly based on polymethacrylates. The two types of bone cement are respectively used in syringes or in dough form and are mainly used for internal fixation of prostheses in total joint replacement surgery. Bone cement is provided in sets of measured sterile powder and sterile liquid, suitable for mixing at the time of implantation. This standard does not involve the hazards of bone cement to patients or users of bone cement when using bone cement. All requirements and all tests apply only to sterile products. 2 Terms and definitions
This standard uses the following terms and definitions.
Unit of cement
One package or bottle of sterile powder and one package or bottle of sterile liquid. NOTE: For bone cements from which the radiopaque agent is supplied separately, the individual sets of bone cement also contain a package or bottle of measured radiopaque powder component. 3 Liquid component
3.1 Appearance
When examined with normal or corrected vision, the liquid shall be free of any particles or other impurities. 3.2 Stability
When tested in accordance with the method described in Appendix A, the increase in the flow time of the liquid sample shall not exceed 10%. 3.3 Precision of contents
When the measurement precision is ±0.1 mL, the volume of each liquid component in the five sets of bone cement shall not exceed 5% of the nominal value on the package [see 9.1b)].
4 Powder component
4.1 Overview
The powder component consists of polymer particles, initiator, and, in the case of radiopaque bone cement, radiopaque agent. In some cases, the radiopaque agent is supplied separately.
4.2 Appearance
When examined with normal or corrected vision, the powder shall be free from lumps and foreign matter. 4.3 Precision of contents
When weighed with an accuracy of ±0.1 g, the mass of each powder component in five sets of bone cement shall not exceed 5 % of the nominal value on the package [see 9.1 b)]. The components tested as described in 3.3 and 4.3 may be subsequently used for the other tests of this standard provided that there is no loss of mass and/or volume and all the requirements of Clauses 3 and 4 are met. 1
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5 Powder-liquid mixtures for use in syringes
The setting characteristics of the powder-liquid mixture and the properties of the bone cement after complete setting shall conform to the values ​​specified in Tables 1 and 2. Table 1 Requirements and test methods for the setting properties of powder-liquid mixtures Closure time
Mixture
For use with syringes
(see Chapter 5)
Use in dough form
Setting time
Maximum deviation from the average value
Average value/min
Test method Average value/minTest method
Maximum deviation/min
Appendix B
Appendix C
Appendix C
Average value/℃
Maximum temperature
Maximum deviation from the average value/℃
Table 2 Requirements and test methods for fully set and polymerized bone cement Average compressive strength
Test method
Appendix E
Powder-liquid mixtures for use in dough form
6.1 Setting characteristics, test methods and requirements
≥1800
Flexural modulus
Test method
Appendix F
Flexural strength
Test method
Appendix C
Appendix C
Test method
Appendix F
When measured by the methods given in Appendix B, Appendix C, Appendix D and Appendix F, the setting characteristics of the powder-liquid mixture and the properties of the bone cement after complete setting shall comply with the values ​​specified in Tables 1 and 2. 6.2 Degree of penetration
When measured by the method described in Appendix D, the average degree of penetration of at least one specimen shall not be less than 2 mm. Solidified and polymerized bone cement
Solidified and polymerized bone cement shall meet the requirements of Table 2. 8 Packaging
8.1 Each component of bone cement shall be packaged and sterilized independently by appropriate methods. Liquid components shall be sterilized by ultrafiltration before being placed in sterile containers. Each component shall be packaged in a double-sealed container, and each set of bone cement shall be further packaged in a container with the information described in 9.1 and the accompanying documents described in 9.2.
Each component of bone cement shall be packaged and sterilized in a double-sealed container, and then packaged in an outer package, which shall be accompanied by the accompanying documents 8.2 When there are two sets of bone cement in one container, the requirements of 8.1 shall be met. 8.3 The packaging material shall not contaminate the contents or cause the contents to be contaminated. During storage and transportation, the packaging shall prevent damage or leakage of the contents and shall be designed to be easy to open and facilitate the sterilization of the contents. 9 Marking
9.1 Single Package Marking
Each single package of bone cement shall be marked with at least the following information: a) This standard number;
b) Description of the contents, including the mass of the powder, the mass or volume of the liquid and the name of each component;2
Name and address of the manufacturer and the supplier other than the manufacturer;c
d) Warning that the contents contain flammable liquids;
YY0459—2003/IS05833:2002
Instructions on the sterility of the contents and warning that bone cement whose packaging has been opened or damaged is not allowed to be used;
f) Instructions on storage below 25°C and instructions on avoiding strong light;g) Batch number of the liquid and powder components and the expiration date of the materials. NOTE Legal requirements for marking may apply in some countries. 9.2
2 Supplementary Documents
The supplementary documents shall contain at least the following information (see Chapter 8): a) instructions for preparing the components and applying the bone cement, including a detailed description of the equipment required and instructions for mixing the entire contents of the package. The instructions should emphasize the importance of minimizing air entrainment when preparing and using the bone cement; b) instructions for introducing and recommending the application of the bone cement, including necessary precautions and the expiration date indicated on the package; instructions for paying attention to the toxicity, harmfulness and irritation of the bone cement and its components during preparation and use; c
d) instructions on how the temperature of the environment or components will shorten or prolong the dough time, application time and setting time of the bone cement; e) instructions on whether the bone cement is to be used in a syringe or in the form of a dough; f) the relative proportions of the powder and liquid components expressed in mass or volume fractions; a warning that the powder and liquid components cannot be re-sterilized; g) instructions on the need to use the entire package at once or discard it and not to reuse it. NOTE: It is helpful to provide a graphical representation of the effect of temperature on the length of each phase of the bone cement curing process based on experimental data from a specific brand of bone cement. 3
YY0459--2003/ISO5833:2002
A.1 Principle
Appendix A
(Informative)
Determination of stability of liquid components
Determine the flow time (viscosity) of the liquid components before and after accelerated aging by heating and calculate the increase in flow time after heating. Determine the liquid components of two sets of bone cement.
A.2 Apparatus
A.2.1 Clean glass U-tube viscometer. A.2.2 Timing device with an accuracy of ±0.1 s. A.2.3 Apparatus for heating the specimen.
A.3 Test conditions
Before the test, the viscometer and the sample are kept at a constant temperature of (23±1)℃ for at least 1h, and then the viscosity is measured at (23±1)℃. A.4 Test steps
A.4.1 Inject the liquid component into the viscometer in the conventional way. A.4.2 Record the flow time (time t) for the curved liquid surface to drop to the equilibrium position. A.4.3 Place the same amount of liquid in a sealed container, heat it in a dark place at (60 ± 2) °C for (48 ± 2) h, then cool it to (23 ± 1) °C and keep it at this temperature for at least 1 h.
A.4.4 Repeat steps A.4.1 and A.4.2 and record the flow time (time t). A.4.5 Repeat steps A.4.1 to A.4.4 for the second set of bone cement liquid components. A.5 Calculation and expression of results
Calculate the percentage change in the flow time of each set of bone cement liquid component △t using the following formula: tb = t × 100%
A.6 Test report
The test report should at least include the following: a) This standard number;
b) The brand of the liquid component (including batch number), the flow time before and after heating;
The percentage change in the flow time of each set of bone cement liquid component. 4
B.1 Principle
Appendix B
(Normative)
YY 0459--2003/ISO 5833:2002
Determination of dough time for bone cement powder-liquid mixtures for use in dough form Mix the bone cement and record the time from the start of mixing until the mixture can be clearly separated from the gloved finger. Determine two or four sets of bone cement.
B.2 Apparatus
B.2.1 Timing device with an accuracy of ±1 s.
B.2.2 Unpowdered surgical latex gloves.
B.2.3 Apparatus recommended by the bone cement manufacturer for mixing bone cement. B.3 Test conditions
Before the test begins, keep the mixing equipment and the contents of the complete set of bone cement at (23 ± 1) °C and a relative humidity (RH) of not less than 40% for at least 2 h. The test is carried out at (23 ± 1) °C and a RH of not less than 40%. B.4 Test procedures
B.4.1 Mix all the materials of a set of bone cement components according to the manufacturer's instructions. When the liquid begins to be added to the powder, start the timing device.
B.4.2 After about 1 min, gently touch the surface of the test mixture with a finger wearing an unpowdered, unwashed surgical latex glove to observe whether fibers are formed between the bone cement and the glove when the finger leaves the bone cement surface. Remove all sticky materials from the glove. B.4.3 Repeat the touch test steps at a maximum interval of 15 seconds, gently mixing the bone cement so that each time you touch the newly exposed surface of the mixture, not the surface that was touched last time, and record the time when the gloved finger can be clearly separated from the bone cement for the first time, which is the dough time of the mixture.
B.4.4 Repeat steps B.4.1 to B.4.3 for the second set of bone cement. B.4.5 If the difference between the two dough times is greater than 30 seconds, repeat steps B.4.1 to B.4.3 with two more sets of bone cement. B.5
Calculation and expression of results
Calculate the average dough time of two or four measured data, round the result to the nearest 15 seconds, and this value is the average dough time. B.6 Test report
The test report should at least include the following: a) This standard number;
b) The brand of bone cement (including batch number); c) The average dough time,
d) The minimum and maximum dough times.
YY 0459--2003/ISO 5833:2002
Appendix C
(Normative Appendix)
Determination of maximum temperature and setting time of powder-liquid mixtures C.1 Principle
Monitor the exothermic reaction occurring during the powder-liquid mixing and record the maximum temperature reached by the mixed mass. The setting time is defined as the time required to reach the median value between the ambient temperature and the maximum temperature. Two or four sets of bone cement are measured. C.2 Apparatus
C.2.1 The dimensions of the male and female molds are as shown in Figure C.1. They are made of polytetrafluoroethylene, polyethylene terephthalate, polyoxymethylene or high-density polyethylene and are equipped with a thermocouple with a wire diameter of approximately 0.5 mm, the end of which is fixed at (3 ± 0.5) mm above the inner surface of the bottom of the female mold. Dimensions: mm
Unless otherwise specified, all dimensional tolerances are ±0.2 mm4
60±0.1
a) Female mold
Wherein,
1-outer ring,
a thermocouple channel,
any polymer screw of suitable size to facilitate the removal of the specimen from the mold, 5Four tapered holes for the excess material to be squeezed out. 8Diameter of the thermocouple hole.
Figure C.1 Mold for determining maximum temperature and solidification time6
b) Male mold
YY 0459-2003/ISO 5833:2002
C.2.2 The device can convert the output signal of the thermocouple into a temperature reading and can continuously record the temperature. The accuracy of the thermocouple and the conversion device is ±0.5℃.
C.2.3 C-clamps, or other devices that can hold the male and female molds together. C.2.4 Timing device with an accuracy of ±0.1 s. C.2.5 Equipment recommended by the bone cement manufacturer for mixing bone cement. C.3 Test conditions
Before the test begins, the mixing equipment and test device and the contents of the bone cement set are kept at (23 ±1)°C and RH not less than 40% for at least 2 h. The test is then carried out at (23 ±1)°C and RH not less than 40%. C.4 Test steps
C.4.1 Record the ambient temperature from the mold thermocouple. C.4.2 Mix all the materials of a set of bone cement components according to the manufacturer's instructions. C.4.3 Start the timing device as soon as the powder and liquid come into contact. C.4.4 Immediately after mixing, fill the female mold with approximately 25 g of bone cement, fix the male mold and clamp it with a C-clamp to ensure a constant volume. A reinforced polymer plate may be used along the bottom of the mould to prevent warping of the mould during polymerisation and expansion of the cement and to remove any cement that may have squeezed out of the mould. C.4.5 Continue to measure the temperature until shortly after the temperature begins to drop. C.4.6 Repeat steps C.4.2 to C.4.5 for the second set of cement. C.4.7 If the two maximum temperatures (see C.5.1) differ by more than 10 °C or the setting times (see C.5.2) differ by more than 1 min, repeat steps C.4.1 to C.4.5 for two more sets of cement. C.5 Calculation and expression of results
C.5.1 Maximum temperature
C.5.1.1 For each set of cement, plot the recorded temperature against time and record the highest temperature reached to the nearest 1 °C as the maximum temperature of the sample.
An example of this graph is shown in Figure C.2.
Figure C.2 Typical curve for determination of maximum temperature and setting time Time, min
YY 0459—2003/ISO 5833:2002
C.5.1.2 Calculate the average of two or four measurements. Round the result to the nearest 1 °C (rounding off values ​​0.5 °C and above) and record this value as the maximum temperature. C.5.2 Setting time
C.5.2.1 For each set of bone cement, determine the setting time, tet, by plotting it in accordance with C.5.1, i.e. measuring the time from the start of mixing until the temperature of the polymerising material reaches the setting temperature T as defined by the following formula: Te = Tmx +Tanb
where:
Tamb - recorded ambient temperature (see C.4.1); maximum temperature reached.
Tmax i
C.5.2.2 Record the tset value to the nearest 5s and calculate the average of two or four measured values ​​ts. Round this result to the nearest 15s and express this value as the setting time.
C.6 Test report
The test report should at least include the following: a)
This standard number,
b) Brand of bone cement (including batch number); c) Average maximum temperature;
d) Each maximum temperature,
e) Average setting time;
f) Each setting time.
D.1 Principle
Appendix D
(Normative Appendix)
YY 04592003/IS0 5833:2002
Determination of the penetration of bone cement powder-liquid mixture used in dough form After the bone cement is mixed, it is pressed into a mold with multiple through holes on the bottom. After the bone cement solidifies, the length of the through holes is measured. Two or four sets of bone cement can be measured.
D.2 Apparatus
D.2.1 The dimensions of the mold and plunger are shown in Figure D.1 and are made of polytetrafluoroethylene, polyethylene terephthalate, polyoxymethylene or high-density polyethylene.
a) Mold
Where:
Outer ring;
X41±0.05
Any polymer screw of suitable size to facilitate the removal of the specimen from the mould. Dimensions: mm
Unless otherwise specified, all dimensions have a tolerance of ±0.2 mm59
b) Column density
Figure D.1 Mould for determining the degree of penetration
D.2.2 Device for applying pressure to the mould.
An instrument for measuring the length of penetration with an accuracy of ±0.5 mm. D.2.3
D.2.4 Equipment proposed by the bone cement manufacturer for mixing bone cement. D.3 Test conditions
Before the test begins, place the mixing equipment and measuring instruments and the contents of the complete set of bone cement at (23 ± 1) °C for at least 2 h. The test is carried out at (23 ± 1) °C.
D.4 Test Procedure
D.4.1 Mix all the ingredients for one set of bone cement according to the manufacturer's instructions. D.4.2 Determine the dough time of the mixture using the procedures given in B.4.2 and B.4.3. Immediately and carefully fill the mould with the mixture and insert the plunger.
D.4.3 Within 1 min ± 10 s after the dough time, apply a force of (49 ± 1) N to the plunger for 1 min ± 2 s. Remove the pressure and allow the bone cement to set.
D.4.4 Remove the set bone cement from the mould and measure the length of cement squeezed into each of the four holes of the mould. This can be determined by subtracting the measured depth of the hole that was not filled with bone cement from the initial hole depth. Calculate the average of the four values ​​to the nearest 0.5 mm. D.4.5 If the average squeeze is less than 2 mm, repeat D.4.1 to D.4.4 with a second set of bone cement. D.5 Test report
The test report shall include at least the following: a) the number of this standard,
b) the brand of bone cement (including batch number); c) the average degree of squeeze for each test sample. 10wwW.bzxz.Net
E.1 Principle
Appendix E
(Normative Appendix)
Determination of compressive strength of bone cement
YY 0459--2003/ISO 5833:2002
After mixing, bone cement is cast into a cylinder and the compressive strength of the cylinder is then determined. Five test bars made from one set of bone cement are measured. E.2 Apparatus
E.2.1 Moulds, end plates and demoulding rods made of stainless steel, with dimensions as shown in Figure E.1; or other devices that can produce bone cement cylinders of appropriate dimensions.
Dimensions: mm
5×Φ6±0.1
a) Through-hole plate
c) End plate (2 pieces)
Unless otherwise specified, all dimensional tolerances are ±0.2 mmb) Mold and plate in fixture
d) Demolding rod
Mold for preparing compressive strength test specimens
C-type clamp or other device that can clamp the mold and end plate together. E.2.2
240 mesh diamond abrasive and block plate.
Demolding agent (optional).
Equipment for mixing bone cement proposed by the bone cement manufacturer. E.2.5
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