微波消解儀校準(zhǔn)規(guī)范試驗(yàn)報(bào)告

1、 微波消解儀校準(zhǔn)規(guī)范試驗(yàn)報(bào)告廣西壯族自治區(qū)計(jì)量檢測研究院2022年7月目 錄TOC o 1-2 h u HYPERLINK l _Toc110517584 1 試驗(yàn)?zāi)康?PAGEREF _Toc110517584 h 1 HYPERLINK l _Toc110517585 2 試驗(yàn)設(shè)備 PAGEREF _Toc110517585 h 1 HYPERLINK l _Toc110517586 3 試驗(yàn)環(huán)境 PAGEREF _Toc110517586 h 1 HYPERLINK l _Toc110517587 4 試驗(yàn)方法 PAGEREF _Toc110517587 h 1 HYPERLINK l

2、_Toc110517588 5 試驗(yàn)結(jié)果 PAGEREF _Toc110517588 h 1 HYPERLINK l _Toc110517589 5.1 試驗(yàn)一：用同一標(biāo)準(zhǔn)器對不同品牌和型號的微波消解儀的試驗(yàn) PAGEREF _Toc110517589 h 1 HYPERLINK l _Toc110517590 5.1.1試驗(yàn)?zāi)康?PAGEREF _Toc110517590 h 2 HYPERLINK l _Toc110517590 5.1.2試驗(yàn)方法 PAGEREF _Toc110517590 h 2 HYPERLINK l _Toc110517593 5.1.3 測試設(shè)備一 PAGEREF

3、 _Toc110517593 h 2 HYPERLINK l _Toc110517596 5.1.4 測試設(shè)備二 PAGEREF _Toc110517596 h 4 HYPERLINK l _Toc110517599 5.1.5 測試設(shè)備三 PAGEREF _Toc110517599 h 6 HYPERLINK l _Toc110517602 5.1.6試驗(yàn)結(jié)果 PAGEREF _Toc110517602 h 9 HYPERLINK l _Toc110517603 5.2 試驗(yàn)二：在不同實(shí)驗(yàn)室用另一臺標(biāo)準(zhǔn)器（同準(zhǔn)確度等級）對微波消解儀的試驗(yàn) PAGEREF _Toc110517603 h 9

4、HYPERLINK l _Toc110517604 5.2.1試驗(yàn)?zāi)康?PAGEREF _Toc110517604 h 9 HYPERLINK l _Toc110517605 5.2.2試驗(yàn)方法 PAGEREF _Toc110517605 h 9 HYPERLINK l _Toc110517608 5.2.3試驗(yàn)結(jié)果 PAGEREF _Toc110517608 h 10 HYPERLINK l _Toc110517609 5.3 試驗(yàn)三：用不同介質(zhì)對同一微波消解儀進(jìn)行校準(zhǔn) PAGEREF _Toc110517609 h 11 HYPERLINK l _Toc110517610 5.3.1試驗(yàn)?zāi)?/p>

5、的 PAGEREF _Toc110517610 h 11 HYPERLINK l _Toc110517611 5.3.2 試驗(yàn)方法 PAGEREF _Toc110517611 h 11 HYPERLINK l _Toc110517612 5.3.3測試設(shè)備一丙三醇試驗(yàn) PAGEREF _Toc110517612 h 11 HYPERLINK l _Toc110517615 5.3.4測試設(shè)備一純水試驗(yàn) PAGEREF _Toc110517615 h 13 HYPERLINK l _Toc110517617 5.3.5測試設(shè)備三丙三醇試驗(yàn) PAGEREF _Toc110517617 h 14 H

6、YPERLINK l _Toc110517620 5.3.6測試設(shè)備三純水試驗(yàn) PAGEREF _Toc110517620 h 16 HYPERLINK l _Toc110517622 5.3.7試驗(yàn)結(jié)果 PAGEREF _Toc110517622 h 18 HYPERLINK l _Toc110517623 5.4 試驗(yàn)四：開始測試時間對微波消解儀溫度參數(shù)測試結(jié)果影響的試驗(yàn) PAGEREF _Toc110517623 h 19 HYPERLINK l _Toc110517624 5.5 試驗(yàn)五：取樣間隔及數(shù)據(jù)量試驗(yàn) PAGEREF _Toc110517624 h 23 HYPERLINK l

7、 _Toc110517630 5.6 試驗(yàn)六：溫度數(shù)據(jù)記錄器數(shù)量對微波消解儀測試結(jié)果影響的試驗(yàn) PAGEREF _Toc110517630 h 29微波消解儀校準(zhǔn)規(guī)范試驗(yàn)報(bào)告1 試驗(yàn)?zāi)康耐ㄟ^試驗(yàn)，驗(yàn)證微波消解儀校準(zhǔn)規(guī)范中規(guī)定的溫度示值誤差、溫度均勻度、溫度波動度、溫度最大過沖量、壓力示值誤差，試驗(yàn)方法的合理性和可行性。2 試驗(yàn)設(shè)備表2-1 校準(zhǔn)裝置技術(shù)指標(biāo)序號名稱測量范圍技術(shù)指標(biāo)1微波專用溫度記錄器（0200）MPE：0.22精密壓力表（0100）MPa0.25級3 試驗(yàn)環(huán)境環(huán)境溫度：（1535） 相對濕度：不大于85%4 試驗(yàn)方法按規(guī)范有關(guān)條文進(jìn)行。5 試驗(yàn)結(jié)果5.1 試驗(yàn)一：用同一標(biāo)準(zhǔn)器對

8、不同品牌和型號的微波消解儀的試驗(yàn)5.1.1試驗(yàn)?zāi)康耐ㄟ^對微波消解儀（溫度示值誤差、溫度均勻度、溫度波動度、溫度最大過沖量）的測量，驗(yàn)證不同廠家、不同型號微波消解儀的溫度示值誤差、溫度均勻度、溫度波動度、最大過沖量等試驗(yàn)。5.1.2試驗(yàn)方法5.1.2.1測量點(diǎn)位置本試驗(yàn)是客戶提供的微波消解儀工作區(qū)尺寸，根據(jù)工作區(qū)尺寸確定記錄器的位置。將微波消解儀及溫度校準(zhǔn)裝置各部件連接完好，按圖5-1-1所示將溫度數(shù)據(jù)記錄器置于微波消解儀轉(zhuǎn)子上的消解罐里，并加入純水，使記錄器完全浸沒于液體中。圖5-1-1 微波消解儀工作區(qū)和測溫點(diǎn)位置示意圖5.1.2.2測試步驟測試是在空載情況下進(jìn)行。按照微波消解儀操作說明書的

9、規(guī)定，設(shè)置溫度數(shù)據(jù)記錄器的數(shù)據(jù)記錄間隔、啟動方式、停止方式等溫度數(shù)據(jù)記錄器運(yùn)行的必要參數(shù)，每個校準(zhǔn)點(diǎn)設(shè)定溫度持續(xù)時間不低于10min，設(shè)置溫度測量裝置的采樣時間間隔最大不超過10s，總采樣時間應(yīng)大于微波消解儀運(yùn)行時間，當(dāng)微波消解儀運(yùn)行至預(yù)設(shè)溫度點(diǎn)（即被校準(zhǔn)溫度點(diǎn)）持續(xù)3min，取之后的數(shù)據(jù)作為校準(zhǔn)數(shù)據(jù)，保證每個溫度數(shù)據(jù)記錄器在測量時間內(nèi)總記錄數(shù)不少于30個。5.1.3 測試設(shè)備一表5-1-1 Multiwave PRO型微波消解儀在150，使用純水介質(zhì)校準(zhǔn)設(shè)備類型接觸式 紅外 光纖設(shè)備圖片設(shè)備型號Multiwave PRO設(shè)備廠家安東帕 Anton Paar消解罐總數(shù)24消解罐規(guī)格容積：50m

10、L 材質(zhì)：PTFE-TFM紅外控溫方式罐平均值 罐最高值 罐最低值試驗(yàn)地點(diǎn)實(shí)驗(yàn)室測試設(shè)備類型長探針 短探針布點(diǎn)圖測試設(shè)備數(shù)量4個測試介質(zhì)純水 丙三醇 其他介質(zhì)量5mL測試溫度150環(huán)境條件17，60%RH5.1.3.1 測試設(shè)備一試驗(yàn)數(shù)據(jù)試驗(yàn)數(shù)據(jù)如以下圖表：表5-1-2 Multiwave PRO型微波消解儀在150，使用純水介質(zhì)校準(zhǔn)數(shù)據(jù)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 測試設(shè)備一校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)結(jié)果：表5-1-3 Multiwave PRO型微波消解儀介質(zhì)為純水時

15、校準(zhǔn)結(jié)果溫度示值誤差/-0.90溫度均勻度/3.99溫度波動度/3.73溫度最大過沖量/4.935.1.4 測試設(shè)備二表5-1-4 MARS 5 PLUS 微波消解儀150、純水介質(zhì)測試數(shù)據(jù)設(shè)備類型接觸式 紅外 光纖設(shè)備圖片設(shè)備型號MARS 5 PLUS設(shè)備廠家CEM消解罐總數(shù)40消解罐規(guī)格容積：55mL 材質(zhì)：改性聚四氟乙烯紅外控溫方式罐平均值 罐最高值 罐最低值試驗(yàn)地點(diǎn)實(shí)驗(yàn)室測試設(shè)備類型長探針 短探針布點(diǎn)圖測試設(shè)備數(shù)量4個測試介質(zhì)純水 丙三醇 其他介質(zhì)量29mL測試溫度150環(huán)境條件19，50%RH5.1.4.1 測試設(shè)備二試驗(yàn)數(shù)據(jù)同理，試驗(yàn)數(shù)據(jù)如以下圖表：表5-1-5 MARS 5 PL

16、US 微波消解儀150、純水介質(zhì)測試數(shù)據(jù)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 測試設(shè)備二校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)結(jié)果：表5-1-6 MARS 5 PLUS 型微波消解儀介質(zhì)為純水時校準(zhǔn)結(jié)果溫度示值誤差/+0.50溫度均勻度/3.69溫度波動度/3.77溫度最大過沖量/3.525.1.5 測試設(shè)備三表5-1-7 MD8H 微波消解儀150、純水介質(zhì)測試數(shù)據(jù)設(shè)備類型接觸式 紅外 光纖設(shè)備圖片設(shè)備型號MD8H設(shè)備廠家奧普樂消解罐總數(shù)16消解罐規(guī)格容積：55mL 材質(zhì)：改性聚四氟乙烯紅

21、外控溫方式罐平均值 罐最高值 罐最低值試驗(yàn)地點(diǎn)實(shí)驗(yàn)室測試設(shè)備類型長探針 短探針布點(diǎn)圖測試設(shè)備數(shù)量4個測試介質(zhì)純水 丙三醇 其他介質(zhì)量10mL測試溫度150環(huán)境條件24，58%RH5.1.5.1 測試設(shè)備三試驗(yàn)數(shù)據(jù)同理，試驗(yàn)數(shù)據(jù)如以下圖表：表5-1-8 MD8H 微波消解儀150、純水介質(zhì)測試數(shù)據(jù)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 測試設(shè)備三校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)結(jié)果：表5-1-9 MD8H 型微波消解儀介質(zhì)為純水時校準(zhǔn)結(jié)果溫度示值誤差/-0.49溫度均勻度/0.82溫度波動

26、度/2.55溫度最大過沖量/2.985.1.6試驗(yàn)結(jié)果經(jīng)過試驗(yàn)，用同一標(biāo)準(zhǔn)器對不同微波消解儀校準(zhǔn)，其溫度示值誤差、溫度均勻度、溫度波動度、溫度最大過沖量均滿足“規(guī)范”中的要求。 5.2 試驗(yàn)二：在不同實(shí)驗(yàn)室用另一臺標(biāo)準(zhǔn)器（同準(zhǔn)確度等級）對微波消解儀的試驗(yàn)5.2.1試驗(yàn)?zāi)康耐ㄟ^對微波消解儀（溫度示值誤差、溫度均勻度、溫度波動度、溫度最大過沖量）的測量，驗(yàn)證不同實(shí)驗(yàn)室用另一臺標(biāo)準(zhǔn)器對微波消解儀的溫度示值誤差、溫度均勻度、溫度波動度、溫度最大過沖量進(jìn)行試驗(yàn)。5.2.2試驗(yàn)方法另外一個實(shí)驗(yàn)室對上述設(shè)備二按照5.1.2的方法進(jìn)行校準(zhǔn)。采用另一套標(biāo)準(zhǔn)器：共4個，1618M354、1618M355、1618

27、M356、1618M357。5.2.2.1 測試設(shè)備二試驗(yàn)數(shù)據(jù)試驗(yàn)數(shù)據(jù)如以下圖表：表5-2-1 MARS 5 PLUS 微波消解儀150、純水介質(zhì)測試數(shù)據(jù)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測試設(shè)備二校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)結(jié)果：表5-2-2 MARS 5 PLUS 型微波消解儀介質(zhì)為純水時校準(zhǔn)結(jié)果溫度示值誤差/+0.04溫度均勻度/3.66溫度波動度/3.05溫度最大過沖量/3.085.2.3試驗(yàn)結(jié)果 經(jīng)過試驗(yàn)，在不同實(shí)驗(yàn)室的另外一臺標(biāo)準(zhǔn)器（同準(zhǔn)確度等級）對同一臺微波消解儀校

32、準(zhǔn)，其溫度示值誤差、溫度均勻度、溫度波動度和溫度最大過沖量均能滿足“規(guī)范”中的要求。 5.3 試驗(yàn)三：用不同介質(zhì)對同一微波消解儀進(jìn)行校準(zhǔn)5.3.1試驗(yàn)?zāi)康挠貌煌橘|(zhì)對同一微波消解儀進(jìn)行校準(zhǔn)，驗(yàn)證介質(zhì)對溫度示值誤差、溫度均勻度、溫度波動度和溫度過沖量的影響。5.3.2 試驗(yàn)方法用丙三醇和純水分別對5.1.2中的測試設(shè)備一和測試設(shè)備三進(jìn)行校準(zhǔn)，驗(yàn)證不同介質(zhì)對溫度示值誤差、度均勻度、溫度波動度和溫度過沖量的影響。5.3.3測試設(shè)備一丙三醇試驗(yàn)表5-3-1 Multiwave PRO型微波消解儀設(shè)備類型接觸式 紅外 光纖設(shè)備圖片設(shè)備型號Multiwave PRO設(shè)備廠家安東帕 Anton Paar消解

33、罐總數(shù)24消解罐規(guī)格容積：50mL 材質(zhì)：PTFE-TFM紅外控溫方式罐平均值 罐最高值 罐最低值試驗(yàn)地點(diǎn)實(shí)驗(yàn)室測試設(shè)備類型長探針 短探針布點(diǎn)圖測試設(shè)備數(shù)量4個測試介質(zhì)純水 丙三醇 其他介質(zhì)量5mL測試溫度150環(huán)境條件17，60%RH5.3.3.1測試設(shè)備一丙三醇試驗(yàn)數(shù)據(jù)用丙三醇對測試設(shè)備一按5.1.2的方法進(jìn)行校準(zhǔn)。表5-3-2 Multiwave PRO型微波消解儀在150，使用丙三醇介質(zhì)校準(zhǔn)數(shù)據(jù)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測試設(shè)備一丙三醇校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)

38、結(jié)果：表5-3-3 Multiwave PRO 型微波消解儀介質(zhì)為丙三醇時校準(zhǔn)結(jié)果溫度示值誤差/-2.59溫度均勻度/2.17溫度波動度/2.60溫度最大過沖量/4.865.3.4測試設(shè)備一純水試驗(yàn)用純水對測試設(shè)備一按5.1.2的方法進(jìn)行校準(zhǔn)。表5-3-4 Multiwave PRO型微波消解儀在150，使用純水介質(zhì)校準(zhǔn)數(shù)據(jù)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測試設(shè)備一純水校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)結(jié)果：表5-3-5 Multiwave PRO型微波消解儀介質(zhì)為純水時校準(zhǔn)結(jié)果溫度

43、示值誤差/-0.90溫度均勻度/3.99溫度波動度/3.73溫度最大過沖量/4.935.3.5測試設(shè)備三丙三醇試驗(yàn)表5-3-6 MD8H型微波消解儀設(shè)備類型接觸式 紅外 光纖設(shè)備圖片設(shè)備型號MD8H設(shè)備廠家奧普樂消解罐總數(shù)16消解罐規(guī)格容積：55mL 材質(zhì)：改性聚四氟乙烯紅外控溫方式罐平均值 罐最高值 罐最低值試驗(yàn)地點(diǎn)實(shí)驗(yàn)室測試設(shè)備類型長探針 短探針布點(diǎn)圖測試設(shè)備數(shù)量4個測試介質(zhì)純水 丙三醇 其他介質(zhì)量8mL測試溫度150環(huán)境條件24，58%RH5.3.5.1測試設(shè)備三丙三醇試驗(yàn)數(shù)據(jù)用丙三醇對測試設(shè)備三按5.1.2的方法進(jìn)行校準(zhǔn)。表5-3-7 MD8H型微波消解儀在150，使用丙三醇介質(zhì)校準(zhǔn)數(shù)

44、據(jù)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測試設(shè)備三丙三醇校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)結(jié)果：表5-3-8 MD8H 型微波消解儀介質(zhì)為丙三醇時校準(zhǔn)結(jié)果溫度示值誤差/-0.77溫度均勻度/1.75溫度波動度/3.03溫度最大過沖量/3.745.3.6測試設(shè)備三純水試驗(yàn)用純水對測試設(shè)備三按5.1.2的方法進(jìn)行校準(zhǔn)。表5-3-9 MD8H 微波消解儀150、使用純水介質(zhì)校準(zhǔn)數(shù)據(jù)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測試設(shè)備三純水校準(zhǔn)項(xiàng)目結(jié)果分析各測試數(shù)據(jù)經(jīng)處理得以下校準(zhǔn)結(jié)果：表5-3-10 MD8H 型微波消解儀介質(zhì)為純水時校準(zhǔn)結(jié)果溫度示值誤差/-0.49溫度均勻度/0.82溫度波動度/2.55溫度最大過沖量/2.985.3.7試驗(yàn)結(jié)果設(shè)備項(xiàng)目純水介質(zhì)丙三醇介質(zhì)Multiwave PRO 型微波消解儀溫度示值誤差/-0.90-2.59溫度均勻度/3.992.17溫度波動度/3.732.60溫度最大過沖量/4.934.86MD8H 型微波消解儀溫度示值誤差/-0.49-0.77溫度均勻度/0.821.75溫度波動度/2.553.03溫度最大過沖量/2.983.74經(jīng)過試驗(yàn)比較可得，對

54、不同廠家、不同型號的2臺微波消解儀分別使用純水和丙三醇介質(zhì)進(jìn)行校準(zhǔn)，介質(zhì)為丙三醇時與介質(zhì)為純水時數(shù)據(jù)結(jié)果差異不大，都能有效的代表設(shè)備實(shí)際工作狀態(tài), 其溫度示值誤差、溫度均勻度、溫度波動度和溫度最大過沖量等均能滿足“規(guī)范”中的要求。使用丙三醇作為校準(zhǔn)介質(zhì)時，需要注意計(jì)量的安全性。因微波消解儀消解罐普遍使用強(qiáng)酸強(qiáng)堿進(jìn)行消解，硝酸與丙三醇發(fā)生反應(yīng)會產(chǎn)生硝酸丙三醇，導(dǎo)致消解罐爆炸。因此在使用丙三醇做介質(zhì)對微波消解儀進(jìn)行校準(zhǔn)時，務(wù)必使用徹底清洗干凈的消解罐。為了安全起見，建議計(jì)量人員使用新消解罐配合標(biāo)準(zhǔn)器進(jìn)行計(jì)量，或使用計(jì)量專用消解罐（不含酸殘留），以保障計(jì)量安全。5.4 試驗(yàn)四：開始測試時間對微波消解

55、儀溫度參數(shù)測試結(jié)果影響的試驗(yàn)經(jīng)過上述幾個試驗(yàn)的數(shù)據(jù)分析，由微波消解儀溫度曲線可以明顯看出，微波消解儀在進(jìn)入設(shè)定工作溫度階段1min3min內(nèi)即可達(dá)到較為穩(wěn)定的狀態(tài)，考慮到不同品牌設(shè)備間的差異，選擇進(jìn)入3min后的數(shù)據(jù)作為校準(zhǔn)數(shù)據(jù)。 下面以四種不同型號的微博消解儀溫度參數(shù)檢測數(shù)據(jù)進(jìn)行說明。測試設(shè)備一：設(shè)備型號：ETHOS UP 標(biāo)準(zhǔn)器編號：1618M746 測試溫度：120圖5-4-1（a）整體曲線圖5-4-1（b）過沖曲線對圖5-4-1結(jié)合微波消解儀設(shè)置程序進(jìn)行分析，微波消解儀于15：06：31開始進(jìn)入消解保溫階段，從15：06：31到15：07：36，溫度并不穩(wěn)定，仍處于溫度過沖期。從15：

56、07：37已經(jīng)進(jìn)入穩(wěn)定階段，進(jìn)入穩(wěn)定階段后，消解溫度存在小幅度波動，但處于平穩(wěn)狀態(tài)。測試備二：設(shè)備型號：MARS 5 PLUS 記錄器編號：1618M746 測試溫度：150圖5-4-2（a）整體曲線圖5-4-2（b）過沖曲線對圖5-4-2結(jié)合微波消解儀設(shè)置程序進(jìn)行分析，微波消解儀于15：46：40開始進(jìn)入消解保溫階段，從15：46：40到15：49：28，溫度并不穩(wěn)定，仍處于溫度過沖期。從15：49：29已經(jīng)進(jìn)入穩(wěn)定階段，進(jìn)入穩(wěn)定階段后，消解溫度存在小幅度波動，但處于平穩(wěn)狀態(tài)。測試設(shè)備三：設(shè)備型號：Multiwave PRO 記錄器編號：1618M328 測試溫度：120圖5-4-3（a）整

57、體曲線圖5-4-3（b）過沖曲線對圖5-4-3結(jié)合微波消解儀設(shè)置程序進(jìn)行分析，微波消解儀于09：57：10開始進(jìn)入消解保溫階段，從09：57：10到09：58：17，溫度并不穩(wěn)定，仍處于溫度過沖期。從09：58：18已經(jīng)進(jìn)入穩(wěn)定階段，進(jìn)入穩(wěn)定階段后，消解溫度存在小幅度波動，但處于平穩(wěn)狀態(tài)。測試設(shè)備四：設(shè)備型號：MD8H 記錄器編號：2 測試溫度：150圖5-4-4（a）整體曲線圖5-4-4（b）整體曲線對圖5-4-4結(jié)合微波消解儀設(shè)置程序進(jìn)行分析，微波消解儀于15：33：20開始進(jìn)入消解保溫階段，從15：33：20到15：33：36，溫度并不穩(wěn)定，仍處于溫度過沖期。從15：33：37已經(jīng)進(jìn)入穩(wěn)

58、定階段，進(jìn)入穩(wěn)定階段后，消解溫度存在小幅度波動，但處于平穩(wěn)狀態(tài)。綜上，對四種不同品牌的微波消解儀溫度數(shù)據(jù)進(jìn)行分析，微波消解儀均在進(jìn)入設(shè)定工作溫度階段1min3min內(nèi)即可達(dá)到較為穩(wěn)定的狀態(tài)，考慮到不同品牌的差異以及數(shù)據(jù)分析的一致性，我們統(tǒng)一選取進(jìn)入設(shè)定溫度階段3min后的數(shù)據(jù)作為校準(zhǔn)數(shù)據(jù)。5.5 試驗(yàn)五：取樣間隔及數(shù)據(jù)量試驗(yàn)根據(jù)微波消解儀實(shí)際工作時間，一般整個消解全過程時間40min（包括升溫階段、保溫階段即消解作用階段、降溫階段），消解作用階段一般持續(xù)時間為10min15min，為保證獲得計(jì)量數(shù)據(jù)量足夠計(jì)算，本實(shí)驗(yàn)設(shè)計(jì)分別設(shè)置標(biāo)準(zhǔn)器采樣間隔為5s、10s、20s、1min，以判斷不同取樣間隔

59、對最終計(jì)量結(jié)果的影響。被測設(shè)備均為MD8H型，測試結(jié)果如圖5-5-1所示。圖5-5-1 MD8H型微波消解儀試驗(yàn)數(shù)據(jù)本次試驗(yàn)數(shù)據(jù)結(jié)果無過沖，消解作用階段開始時間15:29:27，結(jié)束時間15:36:03。5.5.1標(biāo)準(zhǔn)器采樣間隔5s根據(jù)采樣間隔5s選取原始數(shù)據(jù)如表5-5-1所示，測試結(jié)果如表5-5-2。表5-5-1 采樣間隔5s試驗(yàn)數(shù)據(jù)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