CN106596631B - 一种铁矿与氧化铁皮的属性鉴别方法 - Google Patents

一种铁矿与氧化铁皮的属性鉴别方法 Download PDF

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CN106596631B
CN106596631B CN201710076251.1A CN201710076251A CN106596631B CN 106596631 B CN106596631 B CN 106596631B CN 201710076251 A CN201710076251 A CN 201710076251A CN 106596631 B CN106596631 B CN 106596631B
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郭芬
武素茹
赵江勇
李权斌
宋义
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Chemicals Minerals And Metals Testing Center Tianjin Entry-Exit Inspection And Quarantine Bure
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Abstract

本发明涉及一种铁矿与氧化铁皮的属性鉴别方法，该方法主要采用先用X射线荧光光谱仪进行半定量分析，再用差示量热扫描仪对铁矿和氧化铁皮的热学性能进行区分，再结合扫描电镜进行佐证，氧化铁皮在热重分析过程中，呈现明显增重效应，增重在1%以上，在氧气气氛下，其DSC曲线在300℃～400℃呈现的是放热峰，在400℃～1000℃有一个比较宽的放热峰，焓值范围55J/g～600 J/g，热重分析后的样品在扫描电镜下表面呈蜂窝状，与分析前样品的光滑表面有明显的差异，技术效果是明确提出了氧化铁皮与铁矿比对鉴别方法，达到了从源头堵住入境货物易名闯关的目的，为检验检疫、海关提供技术支持，为贸易人提供科学的鉴定报告，确保国境安全，避免环境污染。

Description

一种铁矿与氧化铁皮的属性鉴别方法
技术领域
本发明涉及一种物质属性鉴别方法，特别涉及一种铁矿与氧化铁皮的属性鉴别方法。
背景技术
铁矿是我国大量进口的钢铁工业原料，而氧化铁皮是产生于轧制钢材或锻造钢材的表层，在轧制过程中轧件遇水急剧冷却后钢材表面产生的含铁氧化物，其铁含量高达80%～90 %，因此对这些氧化铁皮的综合利用是非常有必要的。我国对进口氧化铁皮制定了较高的安全、环保要求，并将其纳入限制进口可用作原料的管理范畴，因此按进境废物进行归类，海关H.S编码2619000010，该商品进口需环保许可证，进口废物批准证书等。随着铁矿石进口量的不断增大及高品位铁矿资源的不断减少，国内氧化铁皮应用也越来越广泛，进口氧化铁皮量逐年增加。
近几年我国海关、检验检疫局在对进口铁矿的验放过程中，屡次怀疑铁矿中混有氧化铁皮或烧结矿返矿等商品，如以铁矿品名报关，实际进口货物疑为氧化铁皮、烧结矿、返矿，或铁矿中掺杂该类商品，以逃避监管及关税，处理供（发）货国家的工业垃圾。由于氧化铁皮、烧结矿、返矿中主要元素与铁矿相似，无法仅从各主要元素含量的高低进行区分，为加强铁矿和氧化铁皮的检验监管工作，积极参与国家宏观调控，建立快速鉴别铁矿和氧化铁皮及冶炼废渣的方法，已成为检验监管检测技术一个新的发展方向。
目前已有利用X射线荧光光谱仪、X射线衍射、矿相显微镜、扫描电子显微镜等技术对样品从组成至物相综合对比的研究。上述方法检测结果准确性高，但对实验室的仪器设备、人员要求较高，使得方法的普及上具有一定的局限性。而相反，热重分析方法是在程序控制温度下测量待测样品的质量与温度变化关系的一种热分析技术，从20世纪中叶发展至今已基本成熟，其重要特点是定量性强，已广泛应用于无机物、有机物及聚合物的热分解、金属在高温下受各种气体的腐蚀过程、固态反应、矿物的煅烧和冶炼、液体的蒸馏和汽化、煤、石油和木材的热解过程、含湿量、挥发物及灰分的测定、升华过程、脱水和吸湿等诸多方面的热力学和动力学特征分析研究。所以应用热重分析技术建立铁矿和氧化铁皮的鉴别方法应用而生。
发明内容
鉴于实际工作的需要，本发明提供一种铁矿与氧化铁皮的属性鉴别方法，具体技术方案是，一种铁矿与氧化铁皮的属性鉴别方法，其特征在于：先用X射线荧光光谱仪进行半定量分析，再用差示量热扫描仪对铁矿和氧化铁皮的热学性能进行区分，再结合扫描电镜进行佐证，鉴别步骤如下：（1）、抽取样品数量不少于100g，将抽取的样品逐步缩分、采用压片法破碎至全部通过200目筛网；（2）、全铁含量在50%以上，属于铁矿和氧化铁皮的范围，用X荧光光谱仪对样品进行半定量扫描，初步判断样品是否属于铁矿及氧化铁皮的范围，如果否，则淘汰，如果是，则进行下一步骤的分析；（3）、采取热重分析和差示扫描量热同步热分析对样品进行热学性能分析，a)将样品置于差示量热扫描仪中，在相同的实验条件下对试样同时进行热重与差热分析，得到TGA和DSC曲线，通过对曲线的分析与处理，得到TGA和DSC的特征数据，b）分析以上数据，如经检测样品主要呈现台阶式的明显增重效应，在氧气气氛下，DSC曲线在300℃～400℃呈现的是放热峰，在400℃～1000℃有一个比较宽的放热峰，焓值范围55J/g～600 J/g，则初步判断样品是氧化铁皮，如果存在明显的氧化铁皮的特征峰，则判断样品属性为氧化铁皮，而非铁矿，否则需要进行下一步骤；（4）、采用扫描电镜对经步骤（3）检验后的样品进行样品微观形貌分析， a)按照扫描电镜试样要求制备检测样品，样品被放入电镜中检测并记录特征形貌，b）如果样品形貌结果存在明显的氧化铁皮特性，经热重分析后颗粒表面呈蜂窝状，与分析前样品的光滑表面有明显的差异，这种情况则可确定是氧化铁皮，则判断为氧化铁皮，否则为铁矿。
本发明的有益效果是，明确提出了氧化铁皮与铁矿比对鉴别方法，达到了从源头堵住入境货物易名闯关的目的，为检验检疫、海关提供技术支持，为贸易人提供科学的鉴定报告，确保国境安全，避免环境污染。
附图说明
图1 是105℃下干燥恒重、空气干燥、Mg(NO3)2.6H2O 饱和溶液蒸汽压下平衡的氧化铁皮样品TGA-DSC曲线；
图2是不同速率下的铁矿TGA-DSC曲线峰位的变化；
图3是铁矿在N2和O2 气氛的TGA-DSC曲线；
图4是铁矿的拟合曲线；
图5是氧化铁皮的TGA-DSC曲线；
图6是氧化铁皮的TGA失重量及DSC曲线转变焓。
具体实施方式
如图1、2、3、4、5、6所示，本发明采取的鉴别步骤如下：
（1）、抽取样品数量不少于100g，将抽取的样品逐步缩分、采用压片法破碎至全部通过200目筛网；
（2）、用X荧光光谱仪对样品进行半定量扫描，初步判断样品是否属于铁矿及氧化铁皮的范围，全铁含量在50%以上，属于铁矿和氧化铁皮的范围，如果否，则淘汰，如果是，则进行下一步骤的分析；
（3）、采取热重分析和差示扫描量热同步热分析对样品进行热学性能分析，
a)将样品置于差示量热扫描仪中，在相同的实验条件下对试样同时进行热重与差热分析，得到TGA和DSC曲线，通过对曲线的分析与处理，得到TGA和DSC的特征数据，
b）分析以上数据，如经检测样品主要呈现台阶式的明显增重效应，在氧气气氛下，DSC曲线在300℃～400℃呈现的是放热峰，在400℃～1000℃有一个比较宽的放热峰，焓值范围55J/g～600 J/g，则初步判断样品是氧化铁皮，如果存在明显的氧化铁皮的特征峰，则判断样品属性为氧化铁皮，而非铁矿，否则需要进行下一步骤；
（4）、采用扫描电镜对经步骤（3）检验后的样品进行样品微观形貌分析，
a)按照扫描电镜试样要求制备检测样品，样品被放入电镜中检测并记录特征形貌；
b）如果样品形貌结果存在明显的氧化铁皮特性，经热重分析后颗粒表面呈蜂窝状，与分析前样品的光滑表面有明显的差异，这种情况则可确定是氧化铁皮，则判断为氧化铁皮，否则为铁矿。
实施例1、氧化铁皮的鉴定
首先进行制样，将抽取的100g样品逐步缩分、采用压片法破碎至全部通过200目筛网；
a、经X射线荧光光谱仪半定量分析后，铁含量高达72%，初步判断为氧化铁皮。
b、采用差示量热扫描仪对样品进行热学分析：发现TGA曲线呈现明显的增重效应，在氧气气氛下，DSC曲线在300℃～400℃呈现放热峰，因此判断样品是氧化铁皮。
c、采用扫描电镜观察：对热学分析后的样品进行扫描电镜分析，可以看出表面呈蜂窝状，属于氧化铁皮的特征峰，可以确定该样品为氧化铁皮。
实施例2、对于未知铁矿样品鉴定
对抽取的100g未知样品逐步缩分、采用压片法破碎至全部通过200目筛网。
a、采用 X荧光光谱仪对样品进行半定量扫描，全铁含量在50%以上，属于铁矿和氧化铁皮的范围。
b、将适量样品置于差热分析仪上，对样品进行热重分析，经检测样品主要呈现台阶式的失重效应，失重在3.5%，在氧气气氛下，DSC曲线在300℃～400℃没有明显的放热峰，焓值在-65J/g～386 J/g之间，则初步判断样品是铁矿。
对经上步检测过的样品进行扫描电镜观察：经热重分析后颗粒表面光滑，与分析前样品的光滑表面无明显的差异，这种情况则可确定是铁矿。

Claims (1)

1.一种铁矿与氧化铁皮的属性鉴别方法，其特征在于：先用X射线荧光光谱仪进行半定量分析，再用差示量热扫描仪对铁矿和氧化铁皮的热学性能进行区分，再结合扫描电镜进行佐证，鉴别步骤如下：
（1）、抽取样品数量不少于100g，将抽取的样品逐步缩分、采用压片法破碎至全部通过200目筛网；
（2）、全铁含量在50%以上，属于铁矿和氧化铁皮的范围，用X荧光光谱仪对样品进行半定量扫描，初步判断样品是否属于铁矿及氧化铁皮的范围，如果否，则淘汰，如果是，则进行下一步骤的分析；
（3）、采取热重分析和差示扫描量热同步热分析对样品进行热学性能分析，
a)将样品置于差示量热扫描仪中，在相同的实验条件下对试样同时进行热重与差热分析，得到TGA和DSC曲线，通过对曲线的分析与处理，得到TGA和DSC的特征数据，
b）分析以上数据，如经检测样品TGA曲线主要呈现台阶式的明显增重效应，在氧气气氛下，DSC曲线在300℃～400℃呈现的是放热峰，则初步判断样品是氧化铁皮，在400℃～1000℃有一个比较宽的放热峰，焓值范围412.53J/g～600 J/g，如果存在明显的氧化铁皮的特征峰，则进而判断样品属性为氧化铁皮，而非铁矿，否则需要进行下一步骤；
（4）、采用扫描电镜对经步骤（3）检验后的样品进行样品微观形貌分析，
a)按照扫描电镜试样要求制备检测样品，样品被放入电镜中检测并记录特征形貌；
b）如果样品形貌结果存在明显的氧化铁皮特性，经热重分析后颗粒表面呈蜂窝状，与分析前样品的光滑表面有明显的差异，这种情况则可确定是氧化铁皮，则判断为氧化铁皮，否则为铁矿。
CN201710076251.1A 2017-02-13 2017-02-13 一种铁矿与氧化铁皮的属性鉴别方法 Expired - Fee Related CN106596631B (zh)

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