微波消解仪校准规范试验报告

1、 微波消解仪校准规范试验报告广西壮族自治区计量检测研究院2022年7月目 录TOC o 1-2 h u HYPERLINK l _Toc110517584 1 试验目的 PAGEREF _Toc110517584 h 1 HYPERLINK l _Toc110517585 2 试验设备 PAGEREF _Toc110517585 h 1 HYPERLINK l _Toc110517586 3 试验环境 PAGEREF _Toc110517586 h 1 HYPERLINK l _Toc110517587 4 试验方法 PAGEREF _Toc110517587 h 1 HYPERLINK l

2、_Toc110517588 5 试验结果 PAGEREF _Toc110517588 h 1 HYPERLINK l _Toc110517589 5.1 试验一：用同一标准器对不同品牌和型号的微波消解仪的试验 PAGEREF _Toc110517589 h 1 HYPERLINK l _Toc110517590 5.1.1试验目的 PAGEREF _Toc110517590 h 2 HYPERLINK l _Toc110517590 5.1.2试验方法 PAGEREF _Toc110517590 h 2 HYPERLINK l _Toc110517593 5.1.3 测试设备一 PAGEREF

3、 _Toc110517593 h 2 HYPERLINK l _Toc110517596 5.1.4 测试设备二 PAGEREF _Toc110517596 h 4 HYPERLINK l _Toc110517599 5.1.5 测试设备三 PAGEREF _Toc110517599 h 6 HYPERLINK l _Toc110517602 5.1.6试验结果 PAGEREF _Toc110517602 h 9 HYPERLINK l _Toc110517603 5.2 试验二：在不同实验室用另一台标准器（同准确度等级）对微波消解仪的试验 PAGEREF _Toc110517603 h 9

4、HYPERLINK l _Toc110517604 5.2.1试验目的 PAGEREF _Toc110517604 h 9 HYPERLINK l _Toc110517605 5.2.2试验方法 PAGEREF _Toc110517605 h 9 HYPERLINK l _Toc110517608 5.2.3试验结果 PAGEREF _Toc110517608 h 10 HYPERLINK l _Toc110517609 5.3 试验三：用不同介质对同一微波消解仪进行校准 PAGEREF _Toc110517609 h 11 HYPERLINK l _Toc110517610 5.3.1试验目

5、的 PAGEREF _Toc110517610 h 11 HYPERLINK l _Toc110517611 5.3.2 试验方法 PAGEREF _Toc110517611 h 11 HYPERLINK l _Toc110517612 5.3.3测试设备一丙三醇试验 PAGEREF _Toc110517612 h 11 HYPERLINK l _Toc110517615 5.3.4测试设备一纯水试验 PAGEREF _Toc110517615 h 13 HYPERLINK l _Toc110517617 5.3.5测试设备三丙三醇试验 PAGEREF _Toc110517617 h 14 H

6、YPERLINK l _Toc110517620 5.3.6测试设备三纯水试验 PAGEREF _Toc110517620 h 16 HYPERLINK l _Toc110517622 5.3.7试验结果 PAGEREF _Toc110517622 h 18 HYPERLINK l _Toc110517623 5.4 试验四：开始测试时间对微波消解仪温度参数测试结果影响的试验 PAGEREF _Toc110517623 h 19 HYPERLINK l _Toc110517624 5.5 试验五：取样间隔及数据量试验 PAGEREF _Toc110517624 h 23 HYPERLINK l

7、 _Toc110517630 5.6 试验六：温度数据记录器数量对微波消解仪测试结果影响的试验 PAGEREF _Toc110517630 h 29微波消解仪校准规范试验报告1 试验目的通过试验，验证微波消解仪校准规范中规定的温度示值误差、温度均匀度、温度波动度、温度最大过冲量、压力示值误差，试验方法的合理性和可行性。2 试验设备表2-1 校准装置技术指标序号名称测量范围技术指标1微波专用温度记录器（0200）MPE：0.22精密压力表（0100）MPa0.25级3 试验环境环境温度：（1535） 相对湿度：不大于85%4 试验方法按规范有关条文进行。5 试验结果5.1 试验一：用同一标准器对

8、不同品牌和型号的微波消解仪的试验5.1.1试验目的通过对微波消解仪（温度示值误差、温度均匀度、温度波动度、温度最大过冲量）的测量，验证不同厂家、不同型号微波消解仪的温度示值误差、温度均匀度、温度波动度、最大过冲量等试验。5.1.2试验方法5.1.2.1测量点位置本试验是客户提供的微波消解仪工作区尺寸，根据工作区尺寸确定记录器的位置。将微波消解仪及温度校准装置各部件连接完好，按图5-1-1所示将温度数据记录器置于微波消解仪转子上的消解罐里，并加入纯水，使记录器完全浸没于液体中。图5-1-1 微波消解仪工作区和测温点位置示意图5.1.2.2测试步骤测试是在空载情况下进行。按照微波消解仪操作说明书的

9、规定，设置温度数据记录器的数据记录间隔、启动方式、停止方式等温度数据记录器运行的必要参数，每个校准点设定温度持续时间不低于10min，设置温度测量装置的采样时间间隔最大不超过10s，总采样时间应大于微波消解仪运行时间，当微波消解仪运行至预设温度点（即被校准温度点）持续3min，取之后的数据作为校准数据，保证每个温度数据记录器在测量时间内总记录数不少于30个。5.1.3 测试设备一表5-1-1 Multiwave PRO型微波消解仪在150，使用纯水介质校准设备类型接触式 红外 光纤设备图片设备型号Multiwave PRO设备厂家安东帕 Anton Paar消解罐总数24消解罐规格容积：50m

10、L 材质：PTFE-TFM红外控温方式罐平均值 罐最高值 罐最低值试验地点实验室测试设备类型长探针 短探针布点图测试设备数量4个测试介质纯水 丙三醇 其他介质量5mL测试温度150环境条件17，60%RH5.1.3.1 测试设备一试验数据试验数据如以下图表：表5-1-2 Multiwave PRO型微波消解仪在150，使用纯水介质校准数据Time1618M3421618M3821618M3861618M3900:00:00148.943153.098148.253149.3250:00:10149.132152.371148.220149.0800:00:20147.986151.286148

11、.195148.8760:00:30147.724151.245149.347149.4470:00:40148.739152.143149.820149.6030:00:50149.033152.837149.044149.7330:01:00148.657153.025148.236149.9540:01:10149.099154.053147.461150.5670:01:20149.222152.167148.057151.4090:01:30149.369152.526148.326151.1230:01:40150.236152.722149.093150.3950:01:5014

12、9.614153.433148.669149.6840:02:00149.893154.772149.828150.2150:02:10149.197154.927149.224149.8800:02:20149.354154.851149.363150.7060:02:30149.901154.715149.959150.4930:02:40150.024154.127150.907152.0790:02:50149.713153.490149.142151.3440:03:00149.328153.768148.669151.9400:03:10150.187153.584148.1551

13、50.8530:03:20150.900153.927147.779150.9920:03:30151.252153.075149.436151.0980:03:40150.408153.972150.016152.3000:03:50150.965154.601149.926152.5290:04:00148.657154.641150.506151.7200:04:10148.845154.344150.833151.3190:04:20148.608154.728151.307151.3600:04:30149.082154.483150.220151.1720:04:40149.295

14、154.071149.134151.3600:04:50149.950154.189149.886151.3600:05:00149.320154.715149.412151.3030:05:10149.328154.715150.245152.2760:05:20149.852154.519150.702152.4800:05:30150.384154.883151.176153.6330:05:40151.424154.772149.796152.2925.1.3.2 测试设备一校准项目结果分析各测试数据经处理得以下校准结果：表5-1-3 Multiwave PRO型微波消解仪介质为纯水时

15、校准结果温度示值误差/-0.90温度均匀度/3.99温度波动度/3.73温度最大过冲量/4.935.1.4 测试设备二表5-1-4 MARS 5 PLUS 微波消解仪150、纯水介质测试数据设备类型接触式 红外 光纤设备图片设备型号MARS 5 PLUS设备厂家CEM消解罐总数40消解罐规格容积：55mL 材质：改性聚四氟乙烯红外控温方式罐平均值 罐最高值 罐最低值试验地点实验室测试设备类型长探针 短探针布点图测试设备数量4个测试介质纯水 丙三醇 其他介质量29mL测试温度150环境条件19，50%RH5.1.4.1 测试设备二试验数据同理，试验数据如以下图表：表5-1-5 MARS 5 PL

16、US 微波消解仪150、纯水介质测试数据Time1618M3421618M3821618M3861618M3900:00:00148.392149.253151.277148.7220:00:10148.195149.457150.459148.4770:00:20148.048149.922148.964147.4800:00:30146.845149.718148.629145.9770:00:40148.064150.029148.653146.5320:00:50147.598149.637149.045146.6300:01:00148.032149.743150.001147.56

17、20:01:10147.492150.494150.500147.4070:01:20147.091150.714149.666148.2810:01:30147.688150.061149.854147.8310:01:40147.794151.033149.282148.4610:01:50148.326151.196151.080147.9540:02:00147.222150.763151.555147.0470:02:10147.377150.257150.778147.5050:02:20146.133151.180149.519147.6270:02:30147.320151.6

18、86149.454147.9870:02:40147.541152.503149.536148.5260:02:50147.852151.523150.737148.3870:03:00148.376152.053151.277147.7820:03:10147.844152.592151.816147.8480:03:20146.583152.511150.525148.4360:03:30147.631152.682150.157148.8120:03:40147.508152.731150.116147.6840:03:50148.498153.115151.457149.1640:04

19、:00147.541152.919151.309148.7710:04:10147.303153.058151.571149.5480:04:20146.821152.764151.522148.7140:04:30146.927153.083150.639149.0080:04:40147.222152.021150.991148.4280:04:50147.680151.433149.773148.2810:05:00148.809152.184151.023149.2700:05:10148.728152.813151.072149.5640:05:20147.704153.279152

20、.479148.8450:05:30148.408153.524152.847148.5180:05:40148.728152.192152.699148.9435.1.4.2 测试设备二校准项目结果分析各测试数据经处理得以下校准结果：表5-1-6 MARS 5 PLUS 型微波消解仪介质为纯水时校准结果温度示值误差/+0.50温度均匀度/3.69温度波动度/3.77温度最大过冲量/3.525.1.5 测试设备三表5-1-7 MD8H 微波消解仪150、纯水介质测试数据设备类型接触式 红外 光纤设备图片设备型号MD8H设备厂家奥普乐消解罐总数16消解罐规格容积：55mL 材质：改性聚四氟乙烯红

21、外控温方式罐平均值 罐最高值 罐最低值试验地点实验室测试设备类型长探针 短探针布点图测试设备数量4个测试介质纯水 丙三醇 其他介质量10mL测试温度150环境条件24，58%RH5.1.5.1 测试设备三试验数据同理，试验数据如以下图表：表5-1-8 MD8H 微波消解仪150、纯水介质测试数据Time1618M3421618M3821618M3861618M3900:00:00148.398152.725148.937152.7980:00:10148.521152.560148.978152.6910:00:20148.562152.560148.158152.6170:00:30148.

22、414152.371148.207152.6170:00:40148.316152.355148.060152.4940:00:50148.324152.289148.945152.4120:01:00148.340152.273148.863152.5100:01:10148.283152.150148.757152.5510:01:20148.242152.084148.839152.5600:01:30148.176152.846148.659152.5510:01:40148.069152.682148.601152.4770:01:50148.020152.624148.454152

23、.5510:02:00148.069152.468148.519152.4770:02:10148.045152.443148.552152.4360:02:20148.028152.427148.585152.3950:02:30147.963152.452148.479152.3130:02:40147.881152.706148.470152.1980:02:50147.954152.755148.446152.1740:03:00147.946152.624148.610152.2720:03:10147.881152.517148.659152.3870:03:20148.05315

24、2.723148.528152.2480:03:30148.291152.772148.626152.2560:03:40148.201152.854148.691152.3630:03:50148.266152.051148.634152.5760:04:00148.242152.879148.585152.6090:04:10148.324152.977148.560152.6090:04:20148.332152.854148.708152.6750:04:30148.176152.797148.782152.7730:04:40148.012152.788148.831152.7160

25、:04:50148.061152.879148.954152.7400:05:00148.094152.838148.954152.7890:05:10148.086152.846148.904152.8470:05:20148.168152.870148.790152.8880:05:30148.250152.018148.814152.8310:05:40148.307152.150148.913152.8315.1.5.2 测试设备三校准项目结果分析各测试数据经处理得以下校准结果：表5-1-9 MD8H 型微波消解仪介质为纯水时校准结果温度示值误差/-0.49温度均匀度/0.82温度波动

26、度/2.55温度最大过冲量/2.985.1.6试验结果经过试验，用同一标准器对不同微波消解仪校准，其温度示值误差、温度均匀度、温度波动度、温度最大过冲量均满足“规范”中的要求。 5.2 试验二：在不同实验室用另一台标准器（同准确度等级）对微波消解仪的试验5.2.1试验目的通过对微波消解仪（温度示值误差、温度均匀度、温度波动度、温度最大过冲量）的测量，验证不同实验室用另一台标准器对微波消解仪的温度示值误差、温度均匀度、温度波动度、温度最大过冲量进行试验。5.2.2试验方法另外一个实验室对上述设备二按照5.1.2的方法进行校准。采用另一套标准器：共4个，1618M354、1618M355、1618

27、M356、1618M357。5.2.2.1 测试设备二试验数据试验数据如以下图表：表5-2-1 MARS 5 PLUS 微波消解仪150、纯水介质测试数据Time1618M3541618M3551618M3561618M3570:00:00146.968150.175149.797149.1060:00:10147.778150.878149.626149.3190:00:20148.809150.494149.021148.8200:00:30148.973150.535148.253149.0170:00:40148.285149.498147.771149.2620:00:50148.9

28、81148.804147.886149.5070:01:00147.745148.658150.549149.8340:01:10148.024149.963150.320149.7360:01:20147.500150.437150.574149.8910:01:30147.803149.939149.168150.2760:01:40147.254149.800150.026150.0880:01:50148.302151.351149.903149.1880:02:00147.909150.559151.228148.7300:02:10148.924150.078150.206149.

29、5640:02:20150.005149.465150.745149.3760:02:30150.390150.918149.577149.7200:02:40148.498151.727150.124149.5720:02:50147.844151.302151.334149.7600:03:00146.976151.449150.802150.2270:03:10149.227151.465150.901150.1120:03:20149.243151.645150.230148.9270:03:30149.186152.486151.015149.5810:03:40148.024151

30、.882151.170149.7690:03:50147.631152.004151.416150.7830:04:00148.940152.315150.034149.4330:04:10149.170150.633150.173150.8730:04:20149.227150.755151.563150.7830:04:30147.827151.539152.135151.1590:04:40148.883152.601151.277150.8480:04:50149.014152.674150.623149.9240:05:00149.767151.857151.252149.2450:

31、05:10148.850151.416150.721150.2760:05:20149.202152.797151.064150.2840:05:30149.071153.075150.884150.7250:05:40148.850152.862151.301151.0855.2.2.2测试设备二校准项目结果分析各测试数据经处理得以下校准结果：表5-2-2 MARS 5 PLUS 型微波消解仪介质为纯水时校准结果温度示值误差/+0.04温度均匀度/3.66温度波动度/3.05温度最大过冲量/3.085.2.3试验结果 经过试验，在不同实验室的另外一台标准器（同准确度等级）对同一台微波消解仪校

32、准，其温度示值误差、温度均匀度、温度波动度和温度最大过冲量均能满足“规范”中的要求。 5.3 试验三：用不同介质对同一微波消解仪进行校准5.3.1试验目的用不同介质对同一微波消解仪进行校准，验证介质对温度示值误差、温度均匀度、温度波动度和温度过冲量的影响。5.3.2 试验方法用丙三醇和纯水分别对5.1.2中的测试设备一和测试设备三进行校准，验证不同介质对温度示值误差、度均匀度、温度波动度和温度过冲量的影响。5.3.3测试设备一丙三醇试验表5-3-1 Multiwave PRO型微波消解仪设备类型接触式 红外 光纤设备图片设备型号Multiwave PRO设备厂家安东帕 Anton Paar消解

33、罐总数24消解罐规格容积：50mL 材质：PTFE-TFM红外控温方式罐平均值 罐最高值 罐最低值试验地点实验室测试设备类型长探针 短探针布点图测试设备数量4个测试介质纯水 丙三醇 其他介质量5mL测试温度150环境条件17，60%RH5.3.3.1测试设备一丙三醇试验数据用丙三醇对测试设备一按5.1.2的方法进行校准。表5-3-2 Multiwave PRO型微波消解仪在150，使用丙三醇介质校准数据Time1618M3421618M3821618M3861618M3900:00:00152.029153.508151.137154.0100:00:10153.161153.493150.1

34、59153.7730:00:20152.310154.096151.380153.5860:00:30152.451154.462151.200152.9030:00:40152.265154.184151.627153.4160:00:50150.826152.932150.741153.3430:01:00152.275153.140150.810153.4810:01:10152.174153.788149.701152.8230:01:20152.197154.681149.998152.6930:01:30151.725154.074149.948152.9370:01:40152.

35、634154.410150.641153.2870:01:50152.594154.414150.591152.7260:02:00152.883153.934150.691153.1090:02:10152.050154.390151.790152.6540:02:20152.315153.552151.793152.8350:02:30152.087154.006151.294153.6880:02:40151.965153.810151.769153.6130:02:50152.698154.042151.839152.9690:03:00152.543154.025151.284152

36、.8060:03:10152.703154.191150.891153.5780:03:20152.924154.260151.418153.3590:03:30152.262153.620150.632153.1310:03:40151.714153.895151.558153.2130:03:50151.539154.209150.649152.8950:04:00152.680154.481149.835152.7320:04:10151.769154.204150.442153.1390:04:20152.733154.600151.063153.7570:04:30152.50015

37、4.237150.964154.7730:04:40152.656153.006150.022154.8550:04:50152.558153.059150.400154.2890:05:00151.989152.743149.649154.6590:05:10152.364153.504150.075153.9030:05:20152.451152.885151.294153.7900:05:30152.443153.119149.756154.8230:05:40152.093153.208149.888153.9545.3.3.2测试设备一丙三醇校准项目结果分析各测试数据经处理得以下校准

38、结果：表5-3-3 Multiwave PRO 型微波消解仪介质为丙三醇时校准结果温度示值误差/-2.59温度均匀度/2.17温度波动度/2.60温度最大过冲量/4.865.3.4测试设备一纯水试验用纯水对测试设备一按5.1.2的方法进行校准。表5-3-4 Multiwave PRO型微波消解仪在150，使用纯水介质校准数据Time1618M3421618M3821618M3861618M3900:00:00148.943153.098148.253149.3250:00:10149.132152.371148.220149.0800:00:20147.986151.286148.195148

39、.8760:00:30147.724151.245149.347149.4470:00:40148.739152.143149.820149.6030:00:50149.033152.837149.044149.7330:01:00148.657153.025148.236149.9540:01:10149.099154.053147.461150.5670:01:20149.222152.167148.057151.4090:01:30149.369152.526148.326151.1230:01:40150.236152.722149.093150.3950:01:50149.61415

40、3.433148.669149.6840:02:00149.893154.772149.828150.2150:02:10149.197154.927149.224149.8800:02:20149.354154.851149.363150.7060:02:30149.901154.715149.959150.4930:02:40150.024154.127150.907152.0790:02:50149.713153.490149.142151.3440:03:00149.328153.768148.669151.9400:03:10150.187153.584148.155150.8530

41、:03:20150.900153.927147.779150.9920:03:30151.252153.075149.436151.0980:03:40150.408153.972150.016152.3000:03:50150.965154.601149.926152.5290:04:00148.657154.641150.506151.7200:04:10148.845154.344150.833151.3190:04:20148.608154.728151.307151.3600:04:30149.082154.483150.220151.1720:04:40149.295154.071

42、149.134151.3600:04:50149.950154.189149.886151.3600:05:00149.320154.715149.412151.3030:05:10149.328154.715150.245152.2760:05:20149.852154.519150.702152.4800:05:30150.384154.883151.176153.6330:05:40151.424154.772149.796152.2925.3.4.1测试设备一纯水校准项目结果分析各测试数据经处理得以下校准结果：表5-3-5 Multiwave PRO型微波消解仪介质为纯水时校准结果温度

43、示值误差/-0.90温度均匀度/3.99温度波动度/3.73温度最大过冲量/4.935.3.5测试设备三丙三醇试验表5-3-6 MD8H型微波消解仪设备类型接触式 红外 光纤设备图片设备型号MD8H设备厂家奥普乐消解罐总数16消解罐规格容积：55mL 材质：改性聚四氟乙烯红外控温方式罐平均值 罐最高值 罐最低值试验地点实验室测试设备类型长探针 短探针布点图测试设备数量4个测试介质纯水 丙三醇 其他介质量8mL测试温度150环境条件24，58%RH5.3.5.1测试设备三丙三醇试验数据用丙三醇对测试设备三按5.1.2的方法进行校准。表5-3-7 MD8H型微波消解仪在150，使用丙三醇介质校准数

44、据Time1618M3421618M3821618M3861618M3900:00:00152.334151.533149.000148.5960:00:10152.441151.664149.188148.3840:00:20152.294151.689149.490148.2040:00:30152.179151.517148.878148.1390:00:40151.991151.313148.869148.2860:00:50151.967151.206148.967148.4980:01:00152.081151.190149.123147.7600:01:10152.056151.

45、239148.665147.7520:01:20152.048151.337148.927148.7350:01:30152.269151.795149.213147.8990:01:40152.302152.547149.302148.7680:01:50152.465152.899149.458149.1440:02:00152.539152.882149.286148.4740:02:10152.866152.653149.466147.7930:02:20153.046152.416149.711148.5230:02:30153.259152.637149.629148.5070:0

46、2:40153.332153.087149.637148.6290:02:50153.504153.479149.711148.5390:03:00153.594153.741149.956148.6860:03:10153.398153.430150.013148.4170:03:20153.250153.111149.564148.5310:03:30153.152152.751149.613148.4410:03:40153.234152.580149.850148.5390:03:50153.332152.645149.327147.9100:04:00153.357152.72714

47、9.507148.3710:04:10153.226152.923149.392147.9140:04:20153.226153.209149.539148.6610:04:30153.046153.488149.433148.1060:04:40152.931153.545149.523148.6320:04:50152.792153.373149.564148.2650:05:00152.850153.144149.262148.5340:05:10152.931152.662149.376148.2080:05:20152.989152.653149.490147.6810:05:301

48、52.956152.629149.164149.1220:05:40152.956152.719149.433148.5875.3.5.2测试设备三丙三醇校准项目结果分析各测试数据经处理得以下校准结果：表5-3-8 MD8H 型微波消解仪介质为丙三醇时校准结果温度示值误差/-0.77温度均匀度/1.75温度波动度/3.03温度最大过冲量/3.745.3.6测试设备三纯水试验用纯水对测试设备三按5.1.2的方法进行校准。表5-3-9 MD8H 微波消解仪150、使用纯水介质校准数据Time1618M3421618M3821618M3861618M3900:00:00148.398152.7251

49、48.937152.7980:00:10148.521152.560148.978152.6910:00:20148.562152.560148.158152.6170:00:30148.414152.371148.207152.6170:00:40148.316152.355148.060152.4940:00:50148.324152.289148.945152.4120:01:00148.340152.273148.863152.5100:01:10148.283152.150148.757152.5510:01:20148.242152.084148.839152.5600:01:30

50、148.176152.846148.659152.5510:01:40148.069152.682148.601152.4770:01:50148.020152.624148.454152.5510:02:00148.069152.468148.519152.4770:02:10148.045152.443148.552152.4360:02:20148.028152.427148.585152.3950:02:30147.963152.452148.479152.3130:02:40147.881152.706148.470152.1980:02:50147.954152.755148.44

51、6152.1740:03:00147.946152.624148.610152.2720:03:10147.881152.517148.659152.3870:03:20148.053152.723148.528152.2480:03:30148.291152.772148.626152.2560:03:40148.201152.854148.691152.3630:03:50148.266152.051148.634152.5760:04:00148.242152.879148.585152.6090:04:10148.324152.977148.560152.6090:04:20148.3

52、32152.854148.708152.6750:04:30148.176152.797148.782152.7730:04:40148.012152.788148.831152.7160:04:50148.061152.879148.954152.7400:05:00148.094152.838148.954152.7890:05:10148.086152.846148.904152.8470:05:20148.168152.870148.790152.8880:05:30148.250152.018148.814152.8310:05:40148.307152.1500148.913152

53、.8315.3.6.1测试设备三纯水校准项目结果分析各测试数据经处理得以下校准结果：表5-3-10 MD8H 型微波消解仪介质为纯水时校准结果温度示值误差/-0.49温度均匀度/0.82温度波动度/2.55温度最大过冲量/2.985.3.7试验结果设备项目纯水介质丙三醇介质Multiwave PRO 型微波消解仪温度示值误差/-0.90-2.59温度均匀度/3.992.17温度波动度/3.732.60温度最大过冲量/4.934.86MD8H 型微波消解仪温度示值误差/-0.49-0.77温度均匀度/0.821.75温度波动度/2.553.03温度最大过冲量/2.983.74经过试验比较可得，对

54、不同厂家、不同型号的2台微波消解仪分别使用纯水和丙三醇介质进行校准，介质为丙三醇时与介质为纯水时数据结果差异不大，都能有效的代表设备实际工作状态, 其温度示值误差、温度均匀度、温度波动度和温度最大过冲量等均能满足“规范”中的要求。使用丙三醇作为校准介质时，需要注意计量的安全性。因微波消解仪消解罐普遍使用强酸强碱进行消解，硝酸与丙三醇发生反应会产生硝酸丙三醇，导致消解罐爆炸。因此在使用丙三醇做介质对微波消解仪进行校准时，务必使用彻底清洗干净的消解罐。为了安全起见，建议计量人员使用新消解罐配合标准器进行计量，或使用计量专用消解罐（不含酸残留），以保障计量安全。5.4 试验四：开始测试时间对微波消解

55、仪温度参数测试结果影响的试验经过上述几个试验的数据分析，由微波消解仪温度曲线可以明显看出，微波消解仪在进入设定工作温度阶段1min3min内即可达到较为稳定的状态，考虑到不同品牌设备间的差异，选择进入3min后的数据作为校准数据。 下面以四种不同型号的微博消解仪温度参数检测数据进行说明。测试设备一：设备型号：ETHOS UP 标准器编号：1618M746 测试温度：120图5-4-1（a）整体曲线图5-4-1（b）过冲曲线对图5-4-1结合微波消解仪设置程序进行分析，微波消解仪于15：06：31开始进入消解保温阶段，从15：06：31到15：07：36，温度并不稳定，仍处于温度过冲期。从15：

56、07：37已经进入稳定阶段，进入稳定阶段后，消解温度存在小幅度波动，但处于平稳状态。测试备二：设备型号：MARS 5 PLUS 记录器编号：1618M746 测试温度：150图5-4-2（a）整体曲线图5-4-2（b）过冲曲线对图5-4-2结合微波消解仪设置程序进行分析，微波消解仪于15：46：40开始进入消解保温阶段，从15：46：40到15：49：28，温度并不稳定，仍处于温度过冲期。从15：49：29已经进入稳定阶段，进入稳定阶段后，消解温度存在小幅度波动，但处于平稳状态。测试设备三：设备型号：Multiwave PRO 记录器编号：1618M328 测试温度：120图5-4-3（a）整

57、体曲线图5-4-3（b）过冲曲线对图5-4-3结合微波消解仪设置程序进行分析，微波消解仪于09：57：10开始进入消解保温阶段，从09：57：10到09：58：17，温度并不稳定，仍处于温度过冲期。从09：58：18已经进入稳定阶段，进入稳定阶段后，消解温度存在小幅度波动，但处于平稳状态。测试设备四：设备型号：MD8H 记录器编号：2 测试温度：150图5-4-4（a）整体曲线图5-4-4（b）整体曲线对图5-4-4结合微波消解仪设置程序进行分析，微波消解仪于15：33：20开始进入消解保温阶段，从15：33：20到15：33：36，温度并不稳定，仍处于温度过冲期。从15：33：37已经进入稳

58、定阶段，进入稳定阶段后，消解温度存在小幅度波动，但处于平稳状态。综上，对四种不同品牌的微波消解仪温度数据进行分析，微波消解仪均在进入设定工作温度阶段1min3min内即可达到较为稳定的状态，考虑到不同品牌的差异以及数据分析的一致性，我们统一选取进入设定温度阶段3min后的数据作为校准数据。5.5 试验五：取样间隔及数据量试验根据微波消解仪实际工作时间，一般整个消解全过程时间40min（包括升温阶段、保温阶段即消解作用阶段、降温阶段），消解作用阶段一般持续时间为10min15min，为保证获得计量数据量足够计算，本实验设计分别设置标准器采样间隔为5s、10s、20s、1min，以判断不同取样间隔

59、对最终计量结果的影响。被测设备均为MD8H型，测试结果如图5-5-1所示。图5-5-1 MD8H型微波消解仪试验数据本次试验数据结果无过冲，消解作用阶段开始时间15:29:27，结束时间15:36:03。5.5.1标准器采样间隔5s根据采样间隔5s选取原始数据如表5-5-1所示，测试结果如表5-5-2。表5-5-1 采样间隔5s试验数据Time1618M3421618M3821618M3861618M39015:29:27151.123155.141147.436150.95915:29:32151.189155.240147.600151.37815:29:37151.189154.8871

60、47.354151.27115:29:42151.328155.232147.411151.77215:29:47151.468155.667147.608152.06715:29:52152.010156.480147.887152.52715:29:57151.830156.127147.698152.28915:30:02151.608155.757147.305152.13315:30:07151.246155.741147.076152.06715:30:12151.082155.585147.182151.85415:30:17151.181155.782146.871151.82