冶金分析

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$("#mag-getDinajiShu-175334").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175334&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175334">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175334">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175334');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 辉光放电质谱(GDMS)测定镍基高温合金中痕量镉时,会受到<sup>114</sup>Sn<sup>+</sup>及MoO<sup>+</sup>多原子离子的质谱干扰。本文选择<sup>114</sup>Cd为分析同位素和高分辨模式,采用标准相对灵敏度因子(RSF<sub>Std</sub>)先进行校正后再采用干扰校正方程校正<sup>114</sup>Sn<sup>+</sup>及MoO<sup>+</sup>多原子离子的质谱干扰,实现了辉光放电质谱对镍基高温合金中痕量镉的测定。对仪器参数进行了优化,确定参数如下:放电电流为48 mA,放电气体流速为450 mL/min,预溅射时间为20 min。采用镉认证值小于0.1 μg/g、钼质量分数为3%的镍基变形高温合金标准样品作为空白样品,连续测定11次,以3倍空白标准偏差和10倍空白标准偏差分别计算得到检出限和定量限为0.081 μg/g和0.27 μg/g。采用实验方法测定镍基变形高温合金标准样品中镉含量,测定结果与认定值/标准值吻合性较好,相对标准偏差(RSD,<i>n</i>=6)小于12%。采用实验方法和电感耦合等离子体串联质谱法(ICP-MS/MS)分别对3种镍基高温合金样品中的镉含量进行测定,结果表明,两种方法测定结果基本一致。 </div> </div> </li> <li id="art175335" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175335' class=article_checkbox onclick="hightlightrowaction('art175335')" value='175335' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175335'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012537" target="_blank">电感耦合等离子体质谱法测定镍基合金N06625中痕量硒铈锆钽碲</a> <span mag-component-type="articleStatusIcon" mag-articleId="175335"></span> </div> <div class="j-author">樊鑫, 赵艳兵</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 7-13. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012537">https://doi.org/10.13228/j.boyuan.issn1000-7571.012537</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012537" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175335"></span> <script> $("#mag-getDinajiShu-175335").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175335&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175335">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175335">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175335');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 镍基合金中Se、Ce、Zr、Ta和Te含量对于材料的加工性、热塑性、疲劳性以及蠕变性均有影响,因此其测定具有重要意义。本文以盐酸、过氧化氢、氢氟酸溶解样品,选择<sup>78</sup>Se、<sup>140</sup>Ce、<sup>90</sup>Zr、<sup>181</sup>Ta、<sup>125</sup>Te为测定同位素,采用标准加入法绘制校准曲线以克服基体效应,用<sup>103</sup>Rh校正<sup>78</sup>Se和<sup>90</sup>Zr,<sup>115</sup>In校正<sup>140</sup>Ce、<sup>181</sup>Ta和<sup>125</sup>Te,实现了电感耦合等离子体质谱法(ICP-MS)对镍基合金N06625中痕量Se、Ce、Zr、Ta和Te(质量分数小于0.005%)的同时测定。结果表明,各元素校准曲线的线性相关系数均大于0.999 0,方法的检出限和定量限分别为0.004 5～0.38 μg/g和0.015～1.28 μg/g。采用所建立的方法测定镍基合金N06625样品,5种元素测得结果的相对标准偏差(RSD,<i>n</i>=11)在0.87%～9.9%之间,加标回收率在92%～107%之间。将实验方法应用于镍基合金N06625样品中痕量Se、Ce、Zr、Ta和Te的测定,结果分别与氢化物发生-原子荧光光谱法(HG-AFS)测定Se和Te,电感耦合等离子体原子发射光谱法(ICP-AES)测定Ce和Zr的结果基本吻合。 </div> </div> </li> <li id="art175336" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175336' class=article_checkbox onclick="hightlightrowaction('art175336')" value='175336' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175336'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012516" target="_blank">碱熔-离子色谱法测定低品位萤石尾矿中氟化钙</a> <span mag-component-type="articleStatusIcon" mag-articleId="175336"></span> </div> <div class="j-author">张卓佳, 刘洁, 周姣连, 谢丽芳</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 14-20. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012516">https://doi.org/10.13228/j.boyuan.issn1000-7571.012516</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012516" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175336"></span> <script> $("#mag-getDinajiShu-175336").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175336&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175336">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175336">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175336');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 准确测定低品位萤石尾矿中氟化钙的含量对其综合回收利用工艺的评价和改进意义重大。本实验首先采用波长色散型X射线荧光光谱仪(WDXRF)、X射线衍射仪(XRD)对低品位萤石尾矿样品进行半定量成分分析,确定其中氟元素主要以氟化钙形式存在,且主要含有硅、铝、铁、钙、镁、钾、钠、硫、锰等元素。再以4.0 g氢氧化钾-0.35 g硝酸钾为熔剂,于650 ℃熔融8 min,以热水浸取熔融物,用IC-Na预处理柱分离铝、铁、钙、镁、锰等碱土和过渡金属阳离子,建立了碱熔-离子色谱法测定低品位萤石尾矿中氟化钙的方法。试验表明,经IC-Na预处理柱分离后,试液中铝、铁、钙、镁、锰等阳离子的质量浓度均低于0.1 μg/mL,因此这些元素对测定的干扰可忽略。实验表明,以氟离子质量浓度为横坐标,峰面积响应值为纵坐标绘制校准曲线,在氟离子质量浓度为1～30 μg/mL范围内,校准曲线的线性相关系数为0.999 6。按照实验方法对2个萤石尾矿样品和1个萤石矿标准样品进行测定,并分别加入不同量的高品位萤石矿标准样品进行加标回收试验,加标回收率在96%～104%之间。将实验方法应用于测定低品位萤石尾矿样品和萤石矿标准样品中氟化钙,结果的相对标准偏差(RSD,<i>n</i>=7)为0.54%～1.5%,测定值与离子选择性电极法测定值或标准值相吻合。实验方法可用于测定低品位萤石尾矿中质量分数为5%～60%的氟化钙。 </div> </div> </li> <li id="art175337" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175337' class=article_checkbox onclick="hightlightrowaction('art175337')" value='175337' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175337'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012518" target="_blank">碱溶液提取-流动注射分析仪测定底泥中挥发酚</a> <span mag-component-type="articleStatusIcon" mag-articleId="175337"></span> </div> <div class="j-author">李小辉, 胡新颖, 高志军, 孙慧莹, 于亚辉, 刘春霞</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 21-26. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012518">https://doi.org/10.13228/j.boyuan.issn1000-7571.012518</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012518" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175337"></span> <script> $("#mag-getDinajiShu-175337").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175337&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175337">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175337">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175337');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 准确高效地测定底泥中挥发酚含量,对保护生态环境具有重要的指导意义。控制液固比为15∶1,用10 g/L氢氧化钠溶液以180 r/min振荡15 min对样品中的挥发酚进行浸提,同时加入3.0 g硫酸铜去除样品中硫化物的干扰,实现了流动注射分析法对底泥中挥发酚的测定。结果表明,挥发酚质量浓度在0.02～1.0 mg/L范围内与其对应的峰面积呈线性关系,线性相关系数为0.999 9。方法的检出限为0.08 mg/kg,测定下限为0.32 mg/kg。应用实验方法对3个不同挥发酚含量的底泥样品进行测定,结果的相对标准偏差(RSD,<i>n</i>=6)为0.83%～1.4%。选取两种不同类型的底泥样品,分别进行3个含量水平的加标回收试验,加标回收率在 93%～104%之间。分别采用实验方法和标准方法HJ 998—2018中4-氨基安替比林分光光度法对6个底泥样品中挥发酚进行测定,两种方法的分析结果基本一致。 </div> </div> </li> <li id="art175338" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175338' class=article_checkbox onclick="hightlightrowaction('art175338')" value='175338' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175338'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012555" target="_blank">超级微波消解-电感耦合等离子体原子发射光谱法测定锂矿中氧化锂</a> <span mag-component-type="articleStatusIcon" mag-articleId="175338"></span> </div> <div class="j-author">梁悦锋, 颜焯文, 汤满娜, 禤健文, 萧达辉, 何颖贤</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 27-32. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012555">https://doi.org/10.13228/j.boyuan.issn1000-7571.012555</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012555" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175338"></span> <script> $("#mag-getDinajiShu-175338").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175338&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175338">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175338">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175338');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 锂矿中氧化锂含量为影响锂矿价格的关键因素。在对锂矿中氧化锂进行测定时,通常采用常压分解法,存在操作繁琐、消耗酸量较大的问题。实验采用超级微波消解法及1.5 mL硫酸-2.0 mL氢氟酸体系于280 ℃处理样品,消解后继续加热至硫酸冒烟以去除硅及多余的氢氟酸,然后以1.0 mL硫酸、25 mL水加热重新溶解盐类,选择分析线Li 610.365 nm,发射功率0.95 kW,采用电感耦合等离子体原子发射光谱法(ICP-AES)对试液中锂进行测定,建立了超级微波消解-电感耦合等离子体原子发射光谱法测定锂矿中氧化锂的方法。锂质量浓度在0.50~50.0 mg/L范围内与其对应的发射强度呈良好的线性关系,相关系数<i>r</i>为0.999 7;方法中氧化锂的检出限为1.5 mg/kg。按照实验方法测定3个锂矿试样中氧化锂,结果的相对标准偏差(RSD,<i>n</i>=8)为0.92%～2.0%;方法用于测定2个锂矿石标准物质,测定结果与认定值一致。选择两家分析实验室,分别按照实验方法测定锂矿样品中氧化锂,结果相一致。与现行标准方法GB/T 509.1—2008及GB/T 17413.1—2010相比消解时可节省80%氢氟酸用量,适用于进出口锂矿的快速检验通关。 </div> </div> </li> <li id="art175339" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175339' class=article_checkbox onclick="hightlightrowaction('art175339')" value='175339' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175339'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012570" target="_blank">碱熔-电感耦合等离子体原子发射光谱法测定锂辉石中8种元素</a> <span mag-component-type="articleStatusIcon" mag-articleId="175339"></span> </div> <div class="j-author">杨艳辉, 廖仕英, 陈格, 张杰, 蒋娴芳, 陈怡君</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 33-39. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012570">https://doi.org/10.13228/j.boyuan.issn1000-7571.012570</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012570" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175339"></span> <script> $("#mag-getDinajiShu-175339").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175339&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175339">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175339">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175339');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 采用行业标准YS/T 509—2008《锂辉石、锂云母精矿化学分析方法》中第3、4、5、6、7、8、10部分系列方法测定锂辉石中钙、镁、铁、硅、铝、锰、铍、磷,结果准确,但所用试剂种类较多,且过程繁琐。实验采用氢氧化钠于630 ℃熔融15 min对锂辉石进行碱熔处理,再用盐酸(1+3)酸化浸出,分别在各元素最佳分析谱线处,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锂辉石中钙、镁、铁、硅、铝、锰、铍、磷。采用基体匹配法绘制校准曲线消除了基体效应的影响。各元素校准曲线的线性相关系数均在0.999 7以上;各元素的定量限为0.061 5～123.9 μg/g。按照实验方法测定两个锂辉石样品中钙、镁、铁、硅、铝、锰、铍、磷,测定结果的相对标准偏差(RSD,<i>n</i>=7或<i>n</i>=8)均小于2.5%。按照实验方法对锂辉石标准物质中钙、镁、铁、硅、铝、锰、铍、磷进行测定,测定结果的相对误差(RE)为-5.00%～7.31%。 </div> </div> </li> <li id="art175340" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175340' class=article_checkbox onclick="hightlightrowaction('art175340')" value='175340' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175340'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012545" target="_blank">热处理温度和时间对结晶氯化铝分解产物物相变化的影响</a> <span mag-component-type="articleStatusIcon" mag-articleId="175340"></span> </div> <div class="j-author">白健, 曲直, 张云峰, 任旭东</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 40-46. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012545">https://doi.org/10.13228/j.boyuan.issn1000-7571.012545</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012545" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175340"></span> <script> $("#mag-getDinajiShu-175340").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175340&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175340">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175340">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175340');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 本文主要研究热处理温度、热处理时间对结晶氯化铝分解产物物相变化特征的影响。采用电感耦合等离子体原子发射光谱仪(ICP-AES)及金相显微镜分别对结晶氯化铝的成分和微观形貌进行分析探讨,结果表明,结晶氯化铝纯度较高,含有微量的钠和钙等杂质元素,属于斜方晶系结晶。而氧化铝呈不规则椭圆形,粒径在100～210 μm之间。采用热重分析仪和X射线衍射仪(XRD)对分解产物的物相变化特征进行了考察。结果表明:结晶氯化铝在80～100 ℃热处理失去少量自由水,120 min分解率为6.95%,物相仍为结晶氯化铝。150 ℃热处理120 min分解率为35.84%;200 ℃ 热处理120 min分解率为87.31%;600～1 200 ℃分解速度极快,5 min时全部完成分解。结晶氯化铝的分解率与热处理温度和时间成正比关系,热处理温度是主要因素。热处理温度为200～700 ℃时,分解产物物相是ρ-型或者是无定形型氧化铝;800～1 000 ℃分解产物物相以γ-型氧化铝、δ-型氧化铝、η-型氧化铝为主,其中1 000 ℃分解产物出现少量α-氧化铝。当热处理温度达到1 200 ℃时,所有物相都转变为能量最稳定的α-氧化铝相。本研究为结晶氯化铝热处理理论研究及实验室中试设备选型提供数据依据,为结晶氯化铝热处理工艺参数优化提供数据支撑。 </div> </div> </li> <li id="art175341" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175341' class=article_checkbox onclick="hightlightrowaction('art175341')" value='175341' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175341'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012532" target="_blank">电感耦合等离子体原子发射光谱法测定IN718镍基高温合金中铌的不确定度评定及快速评定方法分析</a> <span mag-component-type="articleStatusIcon" mag-articleId="175341"></span> </div> <div class="j-author">王祥德, 刘含笑, 柏占明, 顾续盛, 杨雪茹, 刘凯</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 47-54. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012532">https://doi.org/10.13228/j.boyuan.issn1000-7571.012532</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012532" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175341"></span> <script> $("#mag-getDinajiShu-175341").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175341&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175341">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175341">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175341');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 测量不确定度可直观地体现测定过程的质量控制水平,随着国内GB/T 22553等标准的发布实施,Top-down法越来越受到重视。分别基于Top-down法和GUM法对IN718镍基高温合金中铌含量测定的不确定度进行评定和比较,发现以Top-down法中再现性标准差<i>s<sub>R</sub></i>评定的不确定度明显高于GUM法评定的结果。对近年金属材料不确定度评定相关文献进行分析,使用简化Top-down法,利用中间精密度评定的不确定度与GUM法评定的不确定度的比值<i>U</i>(<i>R</i><sub><i>w</i></sub>)/<i>U</i>(<i>w</i>)经稳健统计方法处理,稳健平均值为1.20,稳健标准偏差为0.48,说明两种方法的评定结果一致性良好。与GUM法相比,简化Top-down法无需识别称量、标准物质、重复性等分量,无需进行繁琐的计算与合成,评定过程简单、易操作,该方法的使用能够帮助实验室方便快捷的评定不确定度,促进实验室质量控制水平的提升。 </div> </div> </li> <li id="art175342" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175342' class=article_checkbox onclick="hightlightrowaction('art175342')" value='175342' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175342'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012585" target="_blank">氢化物发生-原子荧光光谱法测定镁及镁合金中砷</a> <span mag-component-type="articleStatusIcon" mag-articleId="175342"></span> </div> <div class="j-author">薛宁, 孙改华</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 55-59. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012585">https://doi.org/10.13228/j.boyuan.issn1000-7571.012585</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012585" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175342"></span> <script> $("#mag-getDinajiShu-175342").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175342&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175342">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175342">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175342');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 随着镁及镁合金应用领域的深入,对其中有害元素砷的检测需求越来越多。本文先分次加入硝酸低温加热溶解样品,后用盐酸调节酸度,加入10 mL硫脲-抗坏血酸溶液使As(Ⅴ)还原为As(Ⅲ),建立了氢化物发生-原子荧光光谱法(HG-AFS)对镁及镁合金中微量砷的测定方法。考虑镁及镁合金具有多种产品组别,如镁铝系、镁锌系、镁锰系、镁锂系、镁稀土系,试验考察了不同量镁基体及这些该镁合金组别内铝、锌、锰、铜、镍、锂、镧、铈、镨、钕、钆、钇、铒、镝等元素在最大量存在时对砷测定的影响。结果表明,镁基体与镁合金中主要合金元素对砷测定产生的干扰均可忽略。实验表明,在砷质量浓度为1.00～10.00 μg/L范围内,砷质量浓度与其对应的荧光强度呈线性关系,校准曲线的相关系数为0.999 7。方法检出限为0.001 4 μg/g,定量限为0.004 2 μg/g。按照实验方法测定3个镁合金样品,并分别加入砷标准溶液进行加标回收试验。测定结果的相对标准偏差(RSD,<i>n</i>=6)在2.4%～5.3%之间,加标回收率在98%～106%之间。方法比对试验表明,实验方法测定结果与电感耦合等离子体质谱法(ICP-MS)相符。 </div> </div> </li> <li id="art175343" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175343' class=article_checkbox onclick="hightlightrowaction('art175343')" value='175343' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175343'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012534" target="_blank">基于碱溶液提取法的地块土壤中铬(Ⅵ)测定方法的优化</a> <span mag-component-type="articleStatusIcon" mag-articleId="175343"></span> </div> <div class="j-author">李静, 丁冬梅</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 60-65. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012534">https://doi.org/10.13228/j.boyuan.issn1000-7571.012534</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012534" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175343"></span> <script> $("#mag-getDinajiShu-175343").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175343&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175343">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175343">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175343');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 准确测定地块土壤中铬(Ⅵ)含量对污染地块治理和修复具有重要意义。碱溶液提取-火焰原子吸收光谱法是地块土壤中铬(Ⅵ)测定的主要分析方法之一。文章以地块土壤标准物质和实际样品为研究对象,依次考察了加热方式、搅拌速度、液固比、还原性修复药剂对铬(Ⅵ)测定的影响。结果表明:采用水浴加热方式,地块土壤中的铬(Ⅵ)提取更完全,且测定结果的稳定性优于电加热方式;搅拌速度显著影响铬(Ⅵ)测定结果,持续稳定的中速搅拌效果最佳;通常情况下,液固比为10∶1虽然可以满足常规土壤样品中铬(Ⅵ)的有效提取,然而对于铬(Ⅵ)含量超过校准曲线线性范围上限的地块土壤样品,宜通过减少称样量的方式来确定最佳液固比,以确保结果的准确性和可靠性;还原性修复药剂对铬(Ⅵ)加标试验会形成负干扰,在提取前加入过氧化氢,于室温下超声反应5 min,能够在改变样品基体还原特性的同时维持土壤样品中铬(Ⅲ)化学形态的稳定性,使铬(Ⅵ)加标回收率提高至75.0%～97.5%,有效消除还原性修复药剂对铬(Ⅵ)基体加标回收试验的干扰。 </div> </div> </li> <li id="art175344" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175344' class=article_checkbox onclick="hightlightrowaction('art175344')" value='175344' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175344'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012539" target="_blank">碱熔-硅钼蓝分光光度法测定碳化铬中硅</a> <span mag-component-type="articleStatusIcon" mag-articleId="175344"></span> </div> <div class="j-author">徐华, 曾志平, 施意华, 陈超, 陈家荣</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 66-71. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012539">https://doi.org/10.13228/j.boyuan.issn1000-7571.012539</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012539" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175344"></span> <script> $("#mag-getDinajiShu-175344").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175344&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175344">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175344">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175344');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 准确测定碳化铬中硅含量对其产品质量的控制具有重要意义。实验采用过氧化钠熔融样品,热水浸取后酸化,盐酸挥铬,在一定酸度条件下,硅先与钼酸铵生成硅钼黄,加入草酸-硫酸混合酸消除磷和铁的干扰,最后加入抗坏血酸将硅钼黄还原成硅钼蓝,然后使用分光光度法于波长810 nm处进行测定,建立了碱熔-硅钼蓝分光光度法测定碳化铬中硅的方法。结果表明,当硅质量浓度在0.05～1.20 μg/mL范围内与其相应的吸光度呈良好的线性关系,相关系数为0.999 9;表观摩尔吸光系数为22.41×10<sup>3</sup> L·mol<sup>-1</sup>·cm<sup>-1</sup>。方法检出限为0.001 7%(质量分数,下同),方法定量限为0.005 2%。共存离子干扰试验表明,试液中残余的铬以及样品中的磷和铁不干扰硅的测定。按照实验方法测定3个碳化铬样品中硅,结果的相对标准偏差(RSD,<i>n</i>=9)为0.51%～5.8%。对2个碳化铬样品进行加标回收试验,回收率为97%～102%。 </div> </div> </li> <li id="art175345" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175345' class=article_checkbox onclick="hightlightrowaction('art175345')" value='175345' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175345'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012541" target="_blank">高碘酸钠氧化分光光度法测定硼铁中锰</a> <span mag-component-type="articleStatusIcon" mag-articleId="175345"></span> </div> <div class="j-author">孟伟, 李雅华, 周胜强</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 72-77. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012541">https://doi.org/10.13228/j.boyuan.issn1000-7571.012541</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012541" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175345"></span> <script> $("#mag-getDinajiShu-175345").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175345&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175345">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175345">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175345');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 锰元素可提高硼铁韧性,对锰的准确测定有助于生产更高质量的硼铁基合金材料。采用王水低温溶解后冒高氯酸烟消解样品,在硫磷酸介质中高碘酸钠将锰氧化至七价,于530 nm处采用分光光度法进行测定,建立了一种高碘酸钠氧化分光光度法测定硼铁中锰的方法。分别采用在硫磷酸存在下冒高氯酸烟、冒高氯酸烟后补加硫磷酸、酸溶回渣3种方式处理样品进行试验,结果表明,采用这3种方式溶样,硼铁样品中锰测定结果基本一致,硼铁标准物质/样品中锰测定结果与认定值/标准值相符,其中,冒高氯酸烟后补加硫磷酸法操作最为简单。方法的测定范围为0.050%~1.00%(质量分数,下同),校准曲线的线性相关系数为0.999 99,表观摩尔吸光系数为2.3×10<sup>3</sup> L·mol<sup>-1</sup>·cm<sup>-1</sup>;方法中锰的检出限和定量限分别为0.004%和0.012%。方法用于测定硼铁标准物质和硼铁样品中锰的含量,测得结果的相对标准偏差(<i>n</i>=11)为0.25%～0.46%。按照实验方法测定3个硼铁标准物质/样品和2个硼铁样品中锰含量,标准物质/样品的测定值与认定值/标准值相符,实际样品测定值与酸溶回渣-电感耦合等离子体原子发射光谱法(ICP-AES)测定结果相吻合。 </div> </div> </li> <li id="art175346" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175346' class=article_checkbox onclick="hightlightrowaction('art175346')" value='175346' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175346'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012506" target="_blank">钼对马氏体不锈钢40Cr13Mo全氢罩式退火氧化皮的影响</a> <span mag-component-type="articleStatusIcon" mag-articleId="175346"></span> </div> <div class="j-author">潘红涛, 李照国, 张有余</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 78-83. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012506">https://doi.org/10.13228/j.boyuan.issn1000-7571.012506</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012506" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175346"></span> <script> $("#mag-getDinajiShu-175346").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175346&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175346">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175346">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175346');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 本文对同种工艺生产的40Cr13Mo和40Cr13全氢罩式炉退火钢卷氧化皮样品进行了扫描电镜(SEM)、X射线能谱(EDS),以及X射线衍射(XRD)分析。结果表明:由于Mo的添加,40Cr13Mo不锈钢氧化皮较致密、剥落程度低,内部仅存在一些微小的缺陷,局部存在压应力且强度略高于氧化皮强度;与基体结合区域似胶状、且存在“楔形小凸起”钉扎深度0.81 μm的2FeO·SiO<sub>2</sub>(铁橄榄石);存在氧化皮厚度较小但极差较大,与基体结合面不平整的现象;EDS面扫描Cr元素能量分布趋势与O元素能量分布趋势一致,高能级区域占90%以上且分布在氧化皮的中层、里层,10%的中能级区域分布在氧化皮外围,不存在低能级区域,与基体结合区域Si呈连续中能级宽3 μm条带、条带上伴有3 μm高能级斑块;氧化皮被氢气还原的过程严重滞后,物相以FeCr<sub>2</sub>O<sub>4</sub>和FeO两相为主,两者的含量(质量分数,下同)之和达90.2%,Fe、Cr、Cr<sub>0.7</sub>Fe<sub>0.3</sub>三相的含量仅为9.6%。 </div> </div> </li> <li id="art175347" class="noselectrow"> <div class="article-checkbox"> <INPUT id='thisart_175347' class=article_checkbox onclick="hightlightrowaction('art175347')" value='175347' alt=Select type=checkbox name=pid> <LABEL class=hidelabel for='thisart_175347'>Select</LABEL> </div> <div class="article-l article-w"> <div class="j-title-1"> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012501" target="_blank">基于Paris公式的螺栓疲劳断口定量反推与有限元验证</a> <span mag-component-type="articleStatusIcon" mag-articleId="175347"></span> </div> <div class="j-author">赵睿, 钟振前, 付航</div> <div class="j-volumn-doi"> <span class="j-volumn"> 2024, 44(12): 84-92. </span> <a class="j-doi" href="https://doi.org/10.13228/j.boyuan.issn1000-7571.012501">https://doi.org/10.13228/j.boyuan.issn1000-7571.012501</a> </div> <div class="j-btn"> <span class="article-abstract"> <a class="j-abs" href="http://yjfx.chinamet.cn/gyby/yjfx/CN/10.13228/j.boyuan.issn1000-7571.012501" target="_blank">摘要</a> (<span class="red"> <span id="mag-getDinajiShu-175347"></span> <script> $("#mag-getDinajiShu-175347").load('/gyby/CN/article/getDianJiShu.jsp?articleid=175347&ajax=true'); </script> </span>) </span> <span class="article-pdf"> </span> <span class="richhtml"> </span> <span class="knomap" id="span_visual_article_175347">  <img src="/gyby/images/knowledge_map.png" width="16" height="16" /> <a href="http://yjfx.chinamet.cn/gyby/yjfx/CN/lexeme/showArticleByLexeme.do?articleID=175347">可视化</a> </span> <span class="shoucang">  <img src="/gyby/images/1000-7571/reb.png" width="16" height="16" /> <a href="javascript:;" onclick="collectArticle('175347');"> <span class="shouc">收藏</span> </a> </span> </div> <div class="j-abstract"> 准确预测螺栓的疲劳寿命对于保障工程安全和制定维护计划至关重要。Paris公式是疲劳分析中广泛认可的模型,本研究旨在通过对压力容器中的10.9级螺栓进行疲劳断裂分析来着重探讨Paris公式在疲劳寿命计算中的重要性,并验证Paris公式在预测失效方面的准确性。本文进行了化学元素分析、金相组织分析和电镜观察,通过测量疲劳条带并对疲劳条带宽度进行数据拟合反推两个螺栓断口的疲劳寿命。结果显示#1螺栓的裂纹扩展寿命为17 251个循环,#2螺栓为19 549个循环。有限元模型验证结果表明#1螺栓的裂纹扩展寿命为16 228个循环,#2螺栓为18 525个循环,与实验数据吻合良好,仿真模拟得到的疲劳寿命与计算结果的相对误差不超过6%。研究表明,Paris公式在特定情境下具有准确预测螺栓失效的重要意义,为提高结构件的安全性提供了可靠参考。 </div> </div> </li> </ul> </section>  </div> <div class="tab-pane fade kuang" id="mytab2"> <div mag-component-type="ajaxPage" mag-page-url="http://yjfx.chinamet.cn/gyby/yjfx/CN/online_first?forwardJsp=simple"></div> </div> <div class="tab-pane fade kuang" id="mytab3"> <div mag-component-type="ajaxPage" mag-page-url="http://yjfx.chinamet.cn/gyby/yjfx/CN/archive_by_years?forwardJsp=simple"></div> </div> <div class="tab-pane fade kuang" id="mytab4"> <div mag-component-type="ajaxPage" 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