UNITED STATES
美国
CONSUMER PRODUCT SAFETY COMMISSION
消费品安全委员会
DIRECTORATE FOR LABORATORY SCIENCES
实验室科学理事会
DIVISION OF CHEMISTRY
化学部
10901 DARNESTOWN RD
DARNESTOWN路10901号
GAITHERSBURG, MD 20878
马里兰GAITHERSBURG城20878
Test Method: CPSC-CH-C1001-09.3
测试方法:CPSC-CH-C1001-09.3
Standard Operating Procedure for Determination of Phthalates一直在路上
邻苯二甲酸酯测定的标准操作程序
April 1st, 2010
2010年4月1日
This document provides detailed information on test methods that will be ud by the U.S. Consumer Product Safety Commission’s (CPSC) testing laboratory (LSC) for the analysis of phthalate content in children’s toys and child care articles covered by the standard t forth in the Consumer Product Safety Improvement Act Section 108.
这篇文章详细描述了美国消费品安全委员会(CPSC)测试室(LSC)所涵盖的消费者产品安全改进法案第 108 中规定的儿童玩具和护理品中邻苯二甲酸酯的测试方法。
It has been concluded that in order to protect children from the hazard the Act intended to address, that “concentrations of more than 0.1 percent” must apply per plasticized component part of a children’s toy or child care article1.
它决议出为保护儿童危害行为地方,每一个儿童的玩具或儿童护理品1的部位每种增塑剂“浓度超过 0.1%”。
1 Statement of Policy: Testing of Component Parts with respect to Section 108 of the CPSIA, August 7,
2009 (v/ABOUT/Cpsia/componenttestingpolicy.pdf)
1法律声明:测试部件遵守消费者产品安全改进法案第108款,8月1日,2009
CPSC staff has determined that using an appropriate combination of methods of extraction and analysis prented herein is sufficient to determine the concentration of the
six regulated phthalates in most consumer products. Adjustments may be necessary for
products made from certain materials, and should be bad on sound chemistry and materials science knowledge as well as appropriate solvents for the materials. The general approach is
to dissolve the sample completely in tetrahydrofuran, precipitate any PVC polymer with hexanes, filter and then dilute the solution with cyclohexane, and analyze by Gas Chromatography-Mass Spectrometry (GC-MS).
CPSC确定用一个合适的组合方法能够测定大多数消费品中六种受限制的邻苯二甲酸酯浓度。某些特定的材料产品可能需要调整和基于健康的化学和材料科学知识也要有对材料合适的溶剂。一般通过在四氢呋喃完全溶解它,用正己烷沉淀聚氯乙烯,过滤,然后用环己烷稀释溶液,并用气相色谱质谱联用仪(GC-MS)分析。
Definitions
定义
1.Sample – An individual consumer product or a group of identical consumer products
from a batch to be tested.
样品-从一批货中调出用于检测的个别消费品或一组同样的消费品。
2.Component Part – Individual sub-unit within a product.
组成部件-产品内部的子单位。
3.Laboratory Reagent Blank (LRB) – An aliquot of solvents that is treated exactly as a
sample including exposure to glassware, apparatus and conditions ud for a
particular test, but with no added sample. LRB data are ud to asss contamination
from the laboratory environment.
空白实验试剂(LRB)-一种没有添加样品,同样品一样经过玻璃器皿、设备和条件下测试的一定量溶剂。LRB数据是用于评估从实验环境下受污染的程度。
4.Stock Standard– Phthalate(s) purchad from reputable commercial source at the
highest available purity, ud to prepare calibration standards. Replace before
expiration date.
储备标准-从规范的供应商购买的用于配制校准标准纯邻苯二甲酸酯。在产品有效期前替换掉它。
5.Calibration Standard – Solutions containing the phthalate(s) of interest in
cyclohexane. Each standard should contain 20µg/ml internal standard when
running a 20:1 split injection,or 1µg/ml for splitless injection. A minimum of four
calibration standards are ud. Calibration standards should be prepared as need
from the stock solution and may be stored at room temperature . Record weight of
solutions before and after u to monitor for solvent evaporation. Standards should
be replaced when experimental data demonstrates a decrea in quality or significant loss in solvent weight.
校准标准-在环己烷中含目标邻苯二甲酸酯浓度的溶液。当运行20:1分流进样时,每一个标准溶液必须包含20µg/mL的内标物或使用1µg/mL不分流进样。最少要用四个校准标准。校准标准如果需要,从储备溶液中重新配制并在室温下保存,记录前后溶剂的重量以监控溶剂蒸发。当超过有效期,证明质量或溶剂质量大的流失,需要替换标准溶液。
6.Quality Control Sample (QCS) – Solutions containing known amounts of phthalates
that are ud to evaluate the performance of the analytical instrument system. QCSs
are obtained from a source external to the laboratory and are not made from the Stock Standard solutions. For example, certified reference materials (CRMs) are available from the National Institute of Standards and Technology (NIST), such as tho listed
in the Equipment and Supplies ction below.
质量控制样(QCS)-含有用于评价分析仪器性能的已知一定量的邻苯二甲酸酯溶液。
质量控制样是从本实验室外部获得的,并非是从标准储备溶液配制得来。例如,标准物质(CRM)能从美国标准物质技术研究院得到,例如这些信息在下列仪器和供应品一节中列出。
Equipment and Supplies
仪器和供应品
The materials ud for sampling and analys are as follows:
下列这些材料用于制样和分析:
1. Tetrahydrofuran (C4H8O, THF), GC grade or higher
四氢呋喃(C4H8O, THF),色谱纯或更高
2. Hexane (C6H12), GC grade or higher
正己烷(C6H12),色谱纯或更高
3. Cyclohexane (C6H12), GC grade or higher
环己烷(C6H12),色谱纯或更高
4.Sealable glass vials with PTFE or silicone liner e,size20 ml or larger.
用聚四氟乙烯或硅树脂衬垫密封的20mL玻璃瓶;或更大的。
5.Cryogenic-mill (or suitable alternative to grind samples to powder)
低温研磨机(或合适可用于研磨样品至粉末的)
6.PTFE filters, 0.45 µm.
0.45µm聚四氟乙烯滤器
7.Gas Chromatograph-Mass Spectrometer (GC-MS) with an auto-sampler,
split/splitless inlet, programmable GC oven, and capable of lective ion monitoring.
带自动进样器的气相色谱-质谱联用仪(GC-MS),分流/不分流进样,可编程的柱
箱和可以进行离子选择监测。
8.CRMs containing phthalates (such as NIST SRM 3074)
含邻苯二甲酸酯的标准物质(例如NIST SRM 3074)
9. Benzyl Benzoate (C14H12O2, BB), analytical grade or higher.
苯甲酸苄酯(C14H12O2, BB),分析级或更高
10. Dibutyl Phthalate (C16H22O4, DBP), CAS No. 84-74-2. analytical grade or higher.
邻苯二甲酸二丁酯(C16H22O4, DBP),美国文摘登记号为84-74-2。分析级或更高。官婢
11. Di-(2-ethylhexyl) phthalate (C24H38O4 , DEHP), CAS No. 117-81-7. analytical grade or
higher.
邻苯二甲酸二(2-乙基)己酯(C24H38O4 , DEHP), CAS No. 117-81-7.分析级或更高。
12. Benzyl Butyl Phthalate (C19H20O4, BBP), CAS No. 85-68-7. analytical grade or
higher.
邻苯二甲酸丁苄(C19H20O4, BBP), CAS No. 85-68-7. 分析级或更高
13. Di-n-octyl phthalate (C24H38O4, DnOP), CAS No. 117-84-0. Analytical grade
邻苯二甲酸二正辛酯(C24H38O4, DnOP), CAS No. 117-84-0. 分析级或更高。
14. Diisononyl phthalate (C26H42O4, DINP), CAS No. 28553-12-0/68515-48-0. analytical
grade or higher.
邻苯二甲酸二异壬酯(C26H42O4, DINP), CAS No. 28553-12-0/68515-48-0. 分析级或更高
15.Diisodecyl phthalate (C28H46O4, DIDP), CAS No. 26761-40-0/68515-49-1, analytical
grade or higher.
邻苯二甲酸二异癸酯(C28H46O4, DIDP), CAS No. 26761-40-0/68515-49-1. 分析级
Measurement of Phthalate Concentration
邻苯二甲酸酯含量的测定
The procedure to be ud for all CPSC Compliance Determinations, as described below, consists of three ctions: sample preparation, extraction, and analysis. In addition to the procedure described herein, certain alternate extraction and analysis methods listed below are acceptable to CPSC staff for phthalate content certification testing. Any combination of the ten extraction and five analysis met
hods listed may be ud. However, the CPSC staff’s Sample Preparation method must be performed prior to the alternative extraction and
analysis methods.
程序依据CPSC规定,由如下所述的三个过程组成:样品制备、萃取和分析。在此处所述的
过程外,某些供选用的萃取和分析在下表列出,这些测定邻苯二甲酸酯的方法被CPSC接受
和证实。列出的十种萃取和五种分析方法的组合。然而在可选的萃取和分析方法前,样品制
备方法必须选择CPSC规定的。
Sample Preparation
样品制备
Extraction Method猪舌头煮多长时间能熟
萃取方法
Analysis Method
分析方法
CPSC-CH-C1001-09.3
Health Canada Method C-342 (www.hc-
chim/c-34-eng.php)
加拿大安全方法C-342
搭配销售
CPSC-CH-C1001-09.3
EN 14372:20043
EPA 3540C, Soxhlet Extraction
(v/epawaste/hazard/testmehods/sw
846/pdfs/3540c.pdf)
EPA 3540C,索氏萃取
Health Canada Method
C-34
EPA 3541, Automated Soxhlet Extraction
(v/epawaste/hazard/testmethods/sw
846/pdfs/3541.pdf)
EPA 3541,自动索氏萃取
EPA 3545A, Pressurized Fluid Extraction
(v/epawaste/hazard/testmethods/sw
846/pdfs/3545a.pdf)
团队名称大全
EPA 3545A,加压流动萃取
EN 14372:2004
EPA 3546, Microwave Extraction
(v/epawaste/hazard/testmethods/sw
846/pdfs/3546.pdf)
EPA 3546,微波萃取
EPA 3550C, Ultrasonic Extraction
(v/epawaste/hazard/testmethods/sw
846/pdfs/3550c.pdf)
EPA 3550C,超声萃取
EPA 8270D4 (must be
modified appropriately
to include DINP and
DIDP)
EPA 8270D4(必须适当
的修正DINP和DIDP)
俄罗斯世界杯冠军ASTM D 2124-99 (2004)5
CPSC-CH-C1001-09.3
California Dept. of Toxic Substances Control Method6
加利福利亚有毒物质控制方法6California Dept. of Toxic Substances Control Method
加利福利亚有毒物质控制方法美术画简单又好看
>成绩总结