GB/T 23276-2024 钯化合物分析方法 钯含量的测定 二甲基乙二醛肟析出EDTA络合滴定法和重量法

ICS

77.120.99

CCS

H15

中华人民共和国国家标准

GB/T23276—2024

代替GB/T23276—2009

钯化合物分析方法

钯含量的测定

二甲基乙二醛肟析出EDTA络合滴定法

和重量法

Methodforchemicalanalysisofpalladiumcompounds—

Determinationofpalladiumcontent—

ComplexometrictityationusingbutanedionedioximereleasingEDTAand

gravimetricmethod

2024-09-29发布2025-04-01实施

国家市场监督管理总局

发布

国家标准化管理委员会

GB/T23276—2024

目次

前言

Ⅲ

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1

范围

1

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2

规范性引用文件

1

······················································································

3

术语和定义

1

···························································································

4

方法一：二甲基乙二醛肟析出EDTA络合滴定法

1

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4.1

原理

1

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4.2

试剂或材料

1

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4.3

仪器设备

2

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4.4

样品

2

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4.5

试验步骤

2

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4.6

试验数据处理

3

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4.7

精密度

4

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5

方法二：二甲基乙二醛肟重量法

4

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5.1

原理

4

······························································································

5.2

试剂或材料

4

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5.3

仪器设备

5

·························································································

5.4

样品

5

······························································································

5.5

试验步骤

5

·························································································

5.6

试验数据处理

6

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5.7

精密度

6

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6

试验报告

7

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附录A（资料性）

精密度试验原始数据

8

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Ⅰ

GB/T23276—2024

前言

本文件按照GB/T1.1—2020《标准化工作导则第1部分：标准化文件的结构和起草规则》的规

定起草。

本文件代替GB/T23276—2009《钯化合物分析方法钯量的测定二甲基乙二醛肟析出EDTA络

合滴定法》。与GB/T23276—2009相比，除结构调整和编辑性改动外，主要技术变化如下：

a）更改了测定范围的下限（见第1章，2009年版的第1章）；

b）更改了称样量（见4.5.1，2009年版的6.1）；

c）更改了二甲基乙二醛肟析出EDTA络合滴定法试样的溶解及处理条件（见4.5.4，2009年版的

6.2）；

d）增加了再现性（见4.7.2）；

e）删除了允许差（见2009年版的8.2）；

f）增加了二甲基乙二醛肟重量法（见第5章）。

请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别专利的责任。

本文件由中国有色金属工业协会提出。

本文件由全国有色金属标准化技术委员会（SAC/TC243）归口。

本文件起草单位：贵研检测科技（云南）有限公司、贵研化学材料（云南）有限公司、有色金属技

术经济研究院有限责任公司、云南贵金属实验室有限公司、中船黄冈贵金属有限公司、深圳市中金岭南

有色金属股份有限公司韶关冶炼厂、国标（北京）检验认证有限公司、国合通用（青岛）测试评价有限

公司、成都光明派特贵金属有限公司、江西省君鑫贵金属科技材料有限公司、浙江微通催化新材料有限

公司、东北林业大学、陕西瑞科新材料股份有限公司、广东省科学院工业分析检测中心、云南省贵金属

新材料控股集团股份有限公司。

本文件主要起草人：陶赛祥、金娅秋、陈国华、朱武勋、刘桂华、王丹、向磊、刘朝能、张航波、

杨贞淼、张圣欢、夏江、左鸿毅、胡璇、李甜、王巍、刘含笑、孙阳、林晶、郁丰善、杨帆、刘斌、

王冠群、牛娜、陈立钢、杜冰、史晓妮、周爱玲、周世豪、覃永振、孙祺、杨梅英、鲁瑞智、王川。

本文件于2009年首次发布为GB/T23276—2009，本次为第一次修订。

Ⅲ

GB/T23276—2024

钯化合物分析方法

钯含量的测定

二甲基乙二醛肟析出EDTA络合滴定法

和重量法

警示─使用本文件的人员应有正规实验室的实践经验。本文件并未指出所有可能的安全问题。使

用者有责任采取适当的安全和健康措施，并保证符合国家相关法规规定的条件。使用高氯酸需戴眼镜、

口罩和手套。

1范围

本文件描述了通过二甲基乙二醛肟析出EDTA络合滴定法和重量法测定钯化合物中钯含量的方法。

本文件适用于钯化合物中钯含量的测定，测定范围（质量分数）为4.00%～70.00%。

2规范性引用文件

下列文件中的内容通过文中的规范性引用而构成本文件必不可少的条款。其中，注日期的引用文

件，仅该日期对应的版本适用于本文件；不注日期的引用文件，其最新版本（包括所有的修改单）适用

于本文件。

GB/T6682分析实验室用水规格和试验方法

3术语和定义

本文件没有需要界定的术语和定义。

4方法一：二甲基乙二醛肟析出EDTA络合滴定法

4.1原理

试料用盐酸与硝酸溶解，用高氯酸冒烟分解有机物，加过量EDTA络合钯，加乙酸﹘乙酸钠缓冲溶

液，二甲酚橙作指示剂，在pH≈5.8条件下用锌标准滴定溶液滴定过量EDTA，加二甲基乙二醛肟析出

与钯络合的EDTA，用三氯甲烷萃取丁二酮肟﹘钯沉淀，以锌标准滴定溶液滴定测定钯含量。

4.2试剂或材料

试剂或材料如下。除非另有说明，在分析中仅使用确认为分析纯的试剂。

4.2.1水（符合GB/T6682规定的二级水）。

4.2.2三氯甲烷。

4.2.3高氯酸（ρ=1.77g/mL）。

4.2.4盐酸（ρ=1.19g/mL）。

4.2.5硝酸（ρ=1.42g/mL）。

4.2.6盐酸溶液（1+1）。

4.2.7硝酸溶液（1+1）。

1