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提高直读光谱仪成分分析准确性的方法
<p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;"><span style="line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">直读光谱仪测定结果的精密度与诸多条件紧密相关,直读光谱分析对试验环境温度、湿度的要求较为严格,温度的细微变化会对测定结果产生较大影响。制样质量的好坏直接关系到分析结果的稳定性和准确性,直读光谱分析对块状试样的测定结果准确度较高,对曲率较大的管状试样和直径小于</span>3mm<span style="line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">的棒材,因激发时有效激发面积较小易发生漏气而使测定结果出现较大偏差。直读光谱分析对较高含量的合金元素如铬、镍、铜测定结果的准确度较高,对碳、硫等非金属元素的测定结果准确度和精密度均不够理想。</span></span></p><p style="margin: 0pt; text-align: center; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">&nbsp;<img title="1622684707775446.png" alt="图片1.png" src="/uploads/image/20210603/1622684707775446.png"/></span></p><p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">预燃、冲洗和曝光时间</span>——<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">将冲洗时间降为</span>2s<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">,预燃时间降为</span>6s<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">,火花放电时间降为</span>3s<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">,单样分析时间减少</span>14s<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">,分析速率提高,仪器精密度仍能满足条件。</span></span></p><p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">&nbsp;</span></p><p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">氩气的纯度和流量</span>——<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">氩气流量和压力决定了激发样品时氩气对试样表面放电时的冲击能力,若冲击能力过低,不足以将试样激发过程中产生的气体和形成的化合物冲掉,则会聚集在电极周围抑制试样的继续激发,易形成扩散放电,使放电不稳定,造成分析重复性差;若冲击能力过大,易使火花产生跳动,同样造成放电不稳定,且浪费氩气。为了提高分析结果的精度,用随机所带的超低碳、硫、磷工作曲线来考察氩气流量对测定的影响,结果表明:增加氩气的流量能提高碳测定值的分析精度,但对碳、硫的分析精度影响不大。考虑到氩气流量过大增加分析成本,试验中氩气压力控制在</span>0.3MPa<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">。</span></span></p><p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">&nbsp;</span></p><p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">试样的制备方法</span>——<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">用细砂砂轮机对试样进行表面处理,制样时间短(</span>10s<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">),试样表面平整,纹理清晰,不易污染,且试样不过热,试样分析精密度高,特别是碳和磷的分析精密度明显提高,制样效果明显好于普通砂纸。</span></span></p><p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">&nbsp;</span></p><p style="margin: 0pt; line-height: 1.75em;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: Calibri; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;"><span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">环境温度</span>——<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">夏天检测试样时,试样经常不能完全被激发,碳测定值远远高于实际含量。打开空调将分析室室温调节至</span>25<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">摄氏度左右,再进行试样激发,各元素测定结果准确。其根本原因是温度的变化会使工作曲线产生漂移,故在不同季节温度变化较大时,要尽量保持仪器工作环境恒温,并及时做完全标准化对工作曲线进行校正。每</span>8h<span style="color: rgb(0, 0, 0); line-height: 150%; font-family: 宋体; font-size: 11pt; mso-spacerun: &quot;yes&quot;; mso-fareast-font-family: 宋体; mso-bidi-font-family: &quot;Times New Roman&quot;; mso-font-kerning: 1.0000pt;">做一次标准化校正,分析结果即能满足准确度要求。</span>&nbsp;</span></p><p></p>
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