CPSC-CH-E1001-8.1 测定金属儿童产品（包括儿童金属首饰）中总铅（Pb）的标准操作程序，2010年6月21日修订

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UNITED STATES

CONSUMER PRODUCT SAFETY COMMISSION

DIRECTORATE FOR LABORATORY SCIENCES

DIVISION OF CHEMISTRY

10901 DARNESTOWN RD

GAITHERSBURG, MD 20878

Test Method: CPSC-CH-E1001-8.1

Standard Operating Procedure for Determining Total Lead (Pb) in Metal

Children’s Products (including Children’s Metal Jewelry), Revision

June 21, 2010*

This document provides detailed information on test methodologies that will be used by the U.S.

Consumer Product Safety Commission’s testing laboratory (LSC) in the analysis of children’s

metal products for lead (Pb) content. The set of methods described are used to determine the

total lead content of metal items such as but not limited to children’s metal jewelry. This version

replaces the previously issued Test Method CPSC-CH-E1001-08. The changes are mainly

editorial in nature.

CPSC staff has concluded that these test methods are sufficient to determine lead content in most

metal consumer products. Adjustments may be necessary for products made from certain alloys,

and should be based on sound chemistry knowledge and appropriate acids for the matrix. Test

methods selected shall be those that best demonstrate they can achieve total digestion of the

sample material being analyzed. Test methods shall not be used if they are inconsistent with the

specified application of the test method or do not demonstrate the best performance or

proficiency for achieving total digestion of the sample material.

The methods apply to metal and metal alloy components and have not been recommended by

CPSC staff for other materials that will not dissolve under the conditions specified below, or

when combined with the specified acid(s) results in an inappropriate combination of materials

that would not be consistent with safe laboratory practices.

The general approach is to grind any accessible component part of a sample to a powder, digest

completely in a combination of hot concentrated nitric and hydrochloric acids and analyze by

Inductively Coupled Plasma – Optical Emission Spectroscopy (ICP-OES).

*This is a revision of CPSC Test Method CPSC-CH-E1001-08. This document was prepared by CPSC staff, has not

been reviewed or approved by, and may not necessarily reflect the views of the Commission

-2-

Other analytical methods such as Inductively Coupled Plasma – Mass Spectrometry (ICP-MS)

and Flame Atomic Absorption Spectroscopy (FLAA) and Graphite Furnace Atomic Absorption

Spectroscopy (GFAA) may be used under appropriate conditions as an alternative to ICP-OES

using applicable, recognized analytical techniques for the alternative method.

Definitions

1. Sample – An individual consumer product or a group of identical consumer products

from a batch to be tested.

2. Component part – Individual sub-unit within the total sample. An item such as a bracelet

may be broken into its component parts such as bead, hook, pendant, with those

component parts individually analyzed.

3. Instrument Detection Limit (IDL) – 3 times the standard deviation of 10 replicate

measurements of reagent blank.

4. Method Detection Limit (MDL) - Reagent blank fortified with 2-3 times the IDL. Seven

replicate measurements are made. Calculate the MDL as follows: MDL = t X S, t= 3.14

(99% confidence level for 7 replicates), S= standard deviation.

5. Laboratory Reagent Blank (LRB) – extraction or digestion media used for a particular Pb

test. LRB data are used to assess contamination from the laboratory environment.

6. Calibration Blank – deionized water acidified with nitric acid (3 ml concentrated nitric

acid diluted to 100 ml with deionized water).

7. Stock Standard Solution – 1000 ppm solution of Pb purchased from reputable

commercial source, used to prepare calibration standards. Replace before expiration date.

8. Calibration Standards - Solutions containing 0 to 25 ppm of Pb in 3% nitric acid matrix

are used. A minimum of 4 calibration standards are used. Calibration standards shall be

prepared weekly.

9. Quality Control Sample (QCS) - A solution containing Pb that is used to evaluate the

performance of the instrument system. QCS is obtained from a source external to the

laboratory and Stock Standard Solution.

10. Certified Reference Material (CRM) – CRMs are materials with similar matrix as test

samples with known lead levels. The CRMs are used to verify digestion and analysis

methods. Examples of CRMs are listed in the Equipment and Supplies section below, but

are not limited to only the ones listed.

Equipment and Supplies: The materials used for sampling and analyses are as follows:

1. Nitric Acid, Trace Metal Grade

2. Hydrochloric Acid, Trace Metal Grade

3. Digestion Vessels, 50ml

4. Hot block digester (such as Environmental Express Hot Block)

5. Metal Cutters

6. Distilled Water

7. Microwave Digestion Apparatus

8. Rotary Grinder (Such as Dremel Tool) with carbide burr grinders

9. Orbital Shaker

-3-

10. CRMs for Metals with known lead content, such as NIST SRM 54d, 1728, etc.

11. Internal Standard (such as yttrium, from a stock standard solution of that element,

appropriate to the instrument parameters of the ICP used for the analysis)

I. Total Pb in Metals Digestion

When preparing a sample, the laboratory shall make every effort to assure that the aliquot

removed from a component part of a sample is representative of the component to be tested,

and is free of contamination.

Each unique, accessible component part from a sample is analyzed for total Pb content.

CPSC laboratory staff use either of two methods for determining lead content in metal items.

One method used by CPSC staff is a hot block digestion, based on methodology found in

Canada Product Safety Bureau Method C-02.4.1 This method is equivalent to the procedure

referred to as I. Screening Test for Total Pb Analysis given in the CPSC Standard Operating

Procedure for Determining Lead (Pb) and Its Availability in Children’s Metal Jewelry

2/3/2005 (http://www.cpsc.gov/businfo/pbjeweltest.pdf). Note that the second part of the

reference procedure for determining acid extractability is not applicable for the determination

of total lead content.

The other method used by CPSC staff is a microwave digestion method based on EPA

method 3051A2 (http://www.epa.gov/epawaste/hazard/testmethods/sw846/pdfs/3051a.pdf)

with modifications as described below.

Modifications of these methods may be necessary for certain alloys taking into account

appropriate acids for digestion. Certified reference materials that closely match the alloy of

the tested product should be used to verify accuracy of digestion and analysis methods.

SAMPLE PREPARATION METHODS

Either of two methods outlined below have been found by LSC staff to be suitable for

preparation of metal samples within the scope of this document for subsequent elemental

analysis.

A. Hot Block Method

1. If the item is coated with paint or a similar surface coating (it may contain Pb), the

coating shall be removed and analyzed, separately from the base metal, for lead content

as described in the CPSC Standard Operating Procedure for Determining Lead (Pb) in

Paint (http://www.cpsc.gov/businfo/leadsop.pdf). Care should be taken to remove as

little of the substrate metal as possible.

2. Weigh out 30-100mg of a component part in labeled 50ml digestion vessel. Component

parts of children’s products including metal jewelry items generally weigh several grams

1 Determination of Total Lead in Metallic Consumer Products

2 Microwave Assisted Acid Digestion of Sediments, Sludges, Soils, and Oils

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标签： #金属 #测定

摘要：

本文档详细介绍了美国消费品安全委员会（CPSC）发布的CPSC-CH-E1001-8.1标准操作程序，该程序于2010年6月21日修订，专门用于测定金属儿童产品（包括儿童金属首饰）中的总铅含量。该操作程序为检测机构和制造商提供了标准化的测试方法，涵盖了样品制备、酸消解处理、分析仪器使用（如电感耦合等离子体发射光谱仪或原子吸收光谱仪）以及数据处理与结果报告等关键步骤。通过遵循此SOP，企业能够有效评估产品是否符合美国联邦法规对儿童产品铅含量的强制限值要求，确保儿童金属制品、饰品及玩具的安全合规性，

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CPSC-CH-E1001-8.1 测定金属儿童产品（包括儿童金属首饰）中总铅（Pb）的标准操作程序，2010年6月21日修订

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