(?) (?)石(Shi)墨(Mo)管(Guan)主(Zhu)要(Yao)分(Fen)为(Wei)纵(Zong)向(Xiang)加(Jia)热(Re)和(He)横(Heng)向(Xiang)加(Jia)热(Re)两(Liang)种(Zhong)类(Lei)型(Xing),(?)按(An)性(Xing)能(Neng)可(Ke)分(Fen)为(Wei)普(Pu)通(Tong)石(Shi)墨(Mo)管(Guan)、(?)热(Re)解(Jie)石(Shi)墨(Mo)管(Guan)和(He)平(Ping)台(Tai)石(Shi)墨(Mo)管(Guan),(?)适(Shi)用(Yong)于(Yu)不(Bu)同(Tong)温(Wen)度(Du)范(Fan)围(Wei)的(De)原(Yuan)子(Zi)化(Hua)元(Yuan)素(Su)。(?)
(?) (?)石(Shi)墨(Mo)管(Guan)使(Shi)用(Yong)方(Fang)法(Fa)和(He)要(Yao)点(Dian):(?)
(?) (?)((?)一(Yi))(?)目(Mu)前(Qian)石(Shi)墨(Mo)管(Guan)按(An)加(Jia)热(Re)方(Fang)式(Shi)的(De)不(Bu)同(Tong),(?)有(You)纵(Zong)向(Xiang)加(Jia)热(Re)石(Shi)墨(Mo)管(Guan)和(He)横(Heng)向(Xiang)加(Jia)热(Re)石(Shi)墨(Mo)管(Guan)之(Zhi)分(Fen)。(?)
(?) (?)1.纵(Zong)向(Xiang)加(Jia)热(Re)石(Shi)墨(Mo)管(Guan)有(You):(?)
(?) (?)①(?)标(Biao)准(Zhun)石(Shi)墨(Mo)管(Guan)——适(Shi)用(Yong)于(Yu)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)≤2000℃(?)的(De)元(Yuan)素(Su),(?)如(Ru)Ag、(?)Au、(?)Bi、(?)Cd、(?)Cs、(?)Hg、(?)In、(?)K、(?)Mg、(?)Na、(?)Pb、(?)Rb、(?)Se、(?)Sn、(?)Te、(?)Tl、(?)Zn等(Deng)元(Yuan)素(Su)的(De)测(Ce)试(Shi)。(?)
(?) (?)②(?)平(Ping)台(Tai)镀(Du)层(Ceng)石(Shi)墨(Mo)管(Guan)——适(Shi)用(Yong)于(Yu)中(Zhong)、(?)低(Di)温(Wen)原(Yuan)子(Zi)化(Hua)的(De)元(Yuan)素(Su),(?)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)<(?)2500℃(?)。(?)如(Ru)As、(?)Cu、(?)Fe、(?)Mn、(?)Sb以(Yi)及(Ji)①(?)中(Zhong)提(Ti)到(Dao)的(De)元(Yuan)素(Su)。(?)优(You)点(Dian)是(Shi)精(Jing)度(Du)好(Hao),(?)消(Xiao)除(Chu)干(Gan)扰(Rao)能(Neng)力(Li)强(Qiang)。(?)
(?) (?)③(?)镀(Du)层(Ceng)石(Shi)墨(Mo)管(Guan)——适(Shi)用(Yong)于(Yu)低(Di)、(?)中(Zhong)、(?)高(Gao)温(Wen)原(Yuan)子(Zi)化(Hua)元(Yuan)素(Su)的(De)测(Ce)定(Ding),(?)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)>(?)2500℃(?)。(?)如(Ru)Al、(?)B、(?)Ba、(?)Be、(?)Ca、(?)Co、(?)Cr、(?)Dy、(?)Er、(?)Eu、(?)Ga、(?)Gd、(?)Ge、(?)Ir、(?)La、(?)Li、(?)Mo、(?)Nd、(?)Ni、(?)Os、(?)P、(?)Pd、(?)Pt、(?)Ru、(?)Si、(?)Sm、(?)Sr、(?)Ti、(?)Tm、(?)U、(?)V、(?)Y、(?)Yb。(?)以(Yi)及(Ji)①(?)与(Yu)②(?)中(Zhong)提(Ti)到(Dao)元(Yuan)素(Su)。(?)
(?) (?)2.横(Heng)向(Xiang)加(Jia)热(Re)石(Shi)墨(Mo)管(Guan)由(You)于(Yu)加(Jia)热(Re)方(Fang)式(Shi)不(Bu)同(Tong)于(Yu)纵(Zong)向(Xiang)石(Shi)墨(Mo)管(Guan),(?)通(Tong)电(Dian)后(Hou)整(Zheng)个(Ge)管(Guan)子(Zi)均(Jun)同(Tong)时(Shi)被(Bei)加(Jia)热(Re),(?)不(Bu)存(Cun)在(Zai)温(Wen)度(Du)梯(Ti)度(Du)的(De)影(Ying)响(Xiang),(?)因(Yin)此(Ci)它(Ta)大(Da)大(Da)优(You)于(Yu)纵(Zong)向(Xiang)石(Shi)墨(Mo)管(Guan)。(?)
(?) (?)明(Ming)显(Xian)优(You)点(Dian):(?)
(?) (?)①(?)元(Yuan)素(Su)的(De)灰(Hui)化(Hua)温(Wen)度(Du)与(Yu)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)会(Hui)低(Di)一(Yi)些(Xie)。(?)
(?) (?)②(?)消(Xiao)除(Chu)干(Gan)扰(Rao)能(Neng)力(Li)强(Qiang)。(?)
(?) (?)③(?)灵(Ling)敏(Min)度(Du)更(Geng)高(Gao)。(?)
(?) (?)同(Tong)样(Yang),(?)横(Heng)向(Xiang)加(Jia)热(Re)石(Shi)墨(Mo)管(Guan)也(Ye)有(You)标(Biao)准(Zhun)石(Shi)墨(Mo)管(Guan),(?)平(Ping)台(Tai)镀(Du)层(Ceng)石(Shi)墨(Mo)管(Guan)以(Yi)及(Ji)镀(Du)层(Ceng)石(Shi)墨(Mo)管(Guan)之(Zhi)分(Fen),(?)作(Zuo)用(Yong)与(Yu)纵(Zong)向(Xiang)石(Shi)墨(Mo)管(Guan)类(Lei)似(Si)。(?)但(Dan)成(Cheng)本(Ben)比(Bi)纵(Zong)向(Xiang)管(Guan)要(Yao)高(Gao)许(Xu)多(Duo)。(?)
(?) (?)((?)二(?))(?)当(Dang)石(Shi)墨(Mo)锥(Zhui)已(Yi)使(Shi)用(Yong)过(Guo),(?)在(Zai)装(Zhuang)入(Ru)石(Shi)墨(Mo)管(Guan)之(Zhi)前(Qian)应(Ying)将(Jiang)石(Shi)墨(Mo)锥(Zhui)与(Yu)石(Shi)墨(Mo)管(Guan)接(Jie)触(Chu)处(Chu)用(Yong)挤(Ji)去(Qu)酒(Jiu)精(Jing)的(De)棉(Mian)棒(Bang)进(Jin)行(Xing)清(Qing)洁(Jie)处(Chu)理(Li),(?)而(?)后(Hou)将(Jiang)石(Shi)墨(Mo)管(Guan)装(Zhuang)入(Ru)石(Shi)墨(Mo)炉(Lu)中(Zhong),(?)校(Xiao)正(Zheng)进(Jin)样(Yang)孔(Kong)。(?)
(?) (?)((?)三(San))(?)启(Qi)动(Dong)仪(Yi)器(Qi)事(Shi)先(Xian)设(She)计(Ji)好(Hao)的(De)空(Kong)烧(Shao)程(Cheng)序(Xu),(?)对(Dui)石(Shi)墨(Mo)管(Guan)进(Jin)行(Xing)空(Kong)烧(Shao),(?)使(Shi)石(Shi)墨(Mo)管(Guan)空(Kong)烧(Shao)的(De)吸(Xi)收(Shou)值(Zhi)近(Jin)似(Si)一(Yi)个(Ge)很(Hen)小(Xiao)的(De)吸(Xi)收(Shou)值(Zhi)或(Huo)者(Zhe)为(Wei)零(Ling)。(?)或(Huo)者(Zhe)用(Yong)手(Shou)按(An)动(Dong)在(Zai)2500℃(?)空(Kong)烧(Shao)2-3次(Ci),(?)通(Tong)氩(Ya)气(Qi),(?)时(Shi)间(Jian)2-3秒(Miao)。(?)
(?) (?)((?)四(Si))(?)调(Diao)节(Jie)自(Zi)动(Dong)进(Jin)样(Yang)器(Qi)毛(Mao)细(Xi)管(Guan)插(Cha)入(Ru)石(Shi)墨(Mo)管(Guan)内(Nei)的(De)深(Shen)度(Du)。(?)以(Yi)去(Qu)离(Li)子(Zi)水(Shui)液(Ye)滴(Di)的(De)下(Xia)端(Duan)刚(Gang)刚(Gang)接(Jie)触(Chu)到(Dao)石(Shi)墨(Mo)管(Guan)的(De)内(Nei)壁(Bi),(?)而(?)同(Tong)时(Shi)液(Ye)滴(Di)上(Shang)端(Duan)也(Ye)脱(Tuo)离(Li)进(Jin)样(Yang)毛(Mao)细(Xi)管(Guan),(?)以(Yi)此(Ci)为(Wei)准(Zhun)。(?)现(Xian)在(Zai)原(Yuan)子(Zi)吸(Xi)收(Shou)有(You)多(Duo)种(Zhong)型(Xing)号(Hao)仪(Yi)器(Qi)装(Zhuang)有(You)内(Nei)窥(Kui)镜(Jing),(?)可(Ke)在(Zai)屏(Ping)幕(Mu)上(Shang)清(Qing)楚(Chu)的(De)看(Kan)见(Jian)进(Jin)样(Yang)针(Zhen)进(Jin)行(Xing)调(Diao)节(Jie)。(?)此(Ci)装(Zhuang)置(Zhi)对(Dui)仪(Yi)器(Qi)操(Cao)作(Zuo)者(Zhe)极(Ji)为(Wei)方(Fang)便(Bian),(?)直(Zhi)观(Guan)。(?)可(Ke)方(Fang)便(Bian)调(Diao)节(Jie)测(Ce)试(Shi)元(Yuan)素(Su)的(De)烘(Hong)干(Gan)温(Wen)度(Du)与(Yu)时(Shi)间(Jian)。(?)
(?) (?)((?)五(Wu))(?)石(Shi)墨(Mo)炉(Lu)用(Yong)的(De)保(Bao)护(Hu)气(Qi)体(Ti)应(Ying)该(Gai)采(Cai)用(Yong)高(Gao)纯(Chun)度(Du)((?)≥99.99%)(?)的(De)惰(Duo)性(Xing)气(Qi)体(Ti)氩(Ya)气(Qi)而(?)不(Bu)采(Cai)用(Yong)氮(Dan)气(Qi)。(?)
(?) (?)因(Yin)为(Wei)氮(Dan)气(Qi)使(Shi)极(Ji)大(Da)多(Duo)数(Shu)金(Jin)属(Shu)元(Yuan)素(Su)的(De)吸(Xi)收(Shou)值(Zhi)降(Jiang)低(Di)并(Bing)在(Zai)高(Gao)温(Wen)下(Xia)与(Yu)石(Shi)墨(Mo)管(Guan)的(De)碳(Tan)生(Sheng)成(Cheng)有(You)毒(Du)的(De)CN分(Fen)子(Zi),(?)产(Chan)生(Sheng)严(Yan)重(Zhong)的(De)分(Fen)子(Zi)发(Fa)射(She)和(He)背(Bei)景(Jing)吸(Xi)收(Shou)。(?)同(Tong)时(Shi)石(Shi)墨(Mo)管(Guan)的(De)寿(Shou)命(Ming)也(Ye)比(Bi)使(Shi)用(Yong)氩(Ya)气(Qi)做(Zuo)保(Bao)护(Hu)气(Qi)体(Ti)时(Shi)要(Yao)短(Duan)。(?)所(Suo)以(Yi)不(Bu)用(Yong)氮(Dan)气(Qi)而(?)用(Yong)氩(Ya)气(Qi)。(?)
(?) (?)((?)六(Liu))(?)换(Huan)一(Yi)批(Pi)新(Xin)石(Shi)墨(Mo)管(Guan)测(Ce)定(Ding)时(Shi),(?)必(Bi)须(Xu)先(Xian)进(Jin)行(Xing)待(Dai)测(Ce)元(Yuan)素(Su)的(De)烘(Hong)干(Gan)温(Wen)度(Du)和(He)时(Shi)间(Jian)、(?)灰(Hui)化(Hua)温(Wen)度(Du)和(He)时(Shi)间(Jian)、(?)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)和(He)时(Shi)间(Jian)的(De)选(Xuan)择(Ze)试(Shi)验(Yan),(?)求(Qiu)得(De)待(Dai)测(Ce)元(Yuan)素(Su)的(De)温(Wen)度(Du)和(He)时(Shi)间(Jian)。(?)因(Yin)为(Wei)每(Mei)一(Yi)批(Pi)石(Shi)墨(Mo)管(Guan)的(De)电(Dian)阻(Zu)多(Duo)少(Shao)会(Hui)有(You)差(Cha)别(Bie)。(?)测(Ce)试(Shi)人(Ren)员(Yuan)必(Bi)须(Xu)要(Yao)学(Xue)会(Hui)做(Zuo)灰(Hui)化(Hua)温(Wen)度(Du)与(Yu)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)的(De)曲(Qu)线(Xian)工(Gong)作(Zuo),(?)求(Qiu)得(De)待(Dai)测(Ce)元(Yuan)素(Su)的(De)灰(Hui)化(Hua)温(Wen)度(Du)和(He)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)。(?)利(Li)用(Yong)内(Nei)窥(Kui)镜(Jing)测(Ce)出(Chu)烘(Hong)干(Gan)温(Wen)度(Du)与(Yu)时(Shi)间(Jian)、(?)灰(Hui)化(Hua)温(Wen)度(Du)和(He)时(Shi)间(Jian)。(?)比(Bi)原(Yuan)装(Zhuang)石(Shi)墨(Mo)管(Guan)电(Dian)阻(Zu)大(Da)时(Shi)需(Xu)调(Diao)低(Di)灰(Hui)化(Hua)温(Wen)度(Du)与(Yu)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du),(?)相(Xiang)反(Fan)则(Ze)要(Yao)调(Diao)高(Gao)。(?)
(?) (?)((?)七(Qi))(?)请(Qing)分(Fen)析(Xi)工(Gong)作(Zuo)者(Zhe)切(Qie)记(Ji):(?)待(Dai)测(Ce)样(Yang)品(Pin)溶(Rong)液(Ye)不(Bu)能(Neng)含(Han)有(You)高(Gao)氯(Lu)酸(Suan)、(?)硫(Liu)酸(Suan)等(Deng)强(Qiang)氧(Yang)化(Hua)性(Xing)介(Jie)质(Zhi),(?)否(Fou)则(Ze)对(Dui)石(Shi)墨(Mo)管(Guan)的(De)破(Po)坏(Huai)很(Hen)快(Kuai)且(Qie)严(Yan)重(Zhong)。(?)尤(You)其(Qi)是(Shi)用(Yong)氢(Qing)氟(Fu)酸(Suan)分(Fen)解(Jie)样(Yang)品(Pin),(?)后(Hou)用(Yong)高(Gao)氯(Lu)酸(Suan)赶(Gan)去(Qu)氢(Qing)氟(Fu)酸(Suan)的(De)操(Cao)作(Zuo),(?)高(Gao)氯(Lu)酸(Suan)必(Bi)须(Xu)清(Qing)除(Chu)干(Gan)净(Jing),(?)否(Fou)则(Ze)就(Jiu)会(Hui)出(Chu)现(Xian)开(Kai)始(Shi)标(Biao)准(Zhun)曲(Qu)线(Xian)测(Ce)得(De)很(Hen)好(Hao),(?)测(Ce)样(Yang)品(Pin)溶(Rong)液(Ye)时(Shi)很(Hen)快(Kuai)就(Jiu)出(Chu)现(Xian)吸(Xi)收(Shou)值(Zhi)相(Xiang)差(Cha)很(Hen)大(Da),(?)测(Ce)试(Shi)数(Shu)据(Ju)无(Wu)法(Fa)采(Cai)用(Yong),(?)再(Zai)测(Ce)标(Biao)准(Zhun)溶(Rong)液(Ye)时(Shi)数(Shu)据(Ju)不(Bu)准(Zhun)。(?)也(Ye)可(Ke)将(Jiang)氢(Qing)氟(Fu)酸(Suan)分(Fen)解(Jie)样(Yang)品(Pin)后(Hou)的(De)溶(Rong)液(Ye)蒸(Zheng)干(Gan),(?)然(Ran)后(Hou)用(Yong)稀(Xi)酸(Suan)微(Wei)热(Re)溶(Rong)解(Jie)。(?)
(?) (?)((?)八(Ba))(?)石(Shi)墨(Mo)炉(Lu)测(Ce)定(Ding)元(Yuan)素(Su)时(Shi),(?)吸(Xi)收(Shou)值(Zhi)采(Cai)用(Yong)峰(Feng)面(Mian)积(Ji)形(Xing)式(Shi)而(?)不(Bu)采(Cai)用(Yong)峰(Feng)高(Gao)形(Xing)式(Shi)测(Ce)量(Liang),(?)这(Zhe)样(Yang)带(Dai)来(Lai)较(Jiao)小(Xiao)的(De)误(Wu)差(Cha),(?)而(?)采(Cai)用(Yong)峰(Feng)高(Gao)测(Ce)量(Liang)时(Shi),(?)影(Ying)响(Xiang)因(Yin)素(Su)太(Tai)多(Duo),(?)尤(You)其(Qi)是(Shi)待(Dai)测(Ce)样(Yang)品(Pin)比(Bi)较(Jiao)复(Fu)杂(Za),(?)有(You)影(Ying)响(Xiang)峰(Feng)形(Xing)时(Shi),(?)会(Hui)带(Dai)来(Lai)较(Jiao)大(Da)的(De)误(Wu)差(Cha)。(?)
(?) (?)((?)九(Jiu))(?)测(Ce)定(Ding)时(Shi),(?)烘(Hong)干(Gan)、(?)灰(Hui)化(Hua)、(?)除(Chu)残(Can)阶(Jie)段(Duan),(?)石(Shi)墨(Mo)管(Guan)内(Nei)气(Qi)路(Lu)、(?)外(Wai)气(Qi)路(Lu)必(Bi)须(Xu)通(Tong)氩(Ya)气(Qi)保(Bao)护(Hu);(?)原(Yuan)子(Zi)化(Hua)阶(Jie)段(Duan)时(Shi)内(Nei)气(Qi)路(Lu)停(Ting)气(Qi),(?)或(Huo)小(Xiao)流(Liu)量(Liang)氩(Ya)气(Qi),(?)加(Jia)热(Re)时(Shi)间(Jian)一(Yi)般(Ban)为(Wei)2-3秒(Miao);(?)测(Ce)定(Ding)中(Zhong)、(?)高(Gao)温(Wen)原(Yuan)子(Zi)化(Hua)元(Yuan)素(Su)采(Cai)用(Yong)功(Gong)率(Lu)加(Jia)热(Re),(?)不(Bu)采(Cai)用(Yong)标(Biao)准(Zhun)石(Shi)墨(Mo)管(Guan)或(Huo)平(Ping)台(Tai)石(Shi)墨(Mo)管(Guan)而(?)采(Cai)用(Yong)镀(Du)层(Ceng)石(Shi)墨(Mo)管(Guan)测(Ce)定(Ding)高(Gao)温(Wen)元(Yuan)素(Su);(?)低(Di)温(Wen)原(Yuan)子(Zi)化(Hua)元(Yuan)素(Su)采(Cai)用(Yong)1秒(Miao)或(Huo)0.X秒(Miao)加(Jia)热(Re)。(?)热(Re)除(Chu)残(Can)温(Wen)度(Du)高(Gao)于(Yu)原(Yuan)子(Zi)化(Hua)温(Wen)度(Du)100-200℃(?),(?)加(Jia)热(Re)时(Shi)间(Jian)1-2秒(Miao),(?)内(Nei)外(Wai)通(Tong)氩(Ya)气(Qi),(?)可(Ke)提(Ti)高(Gao)石(Shi)墨(Mo)管(Guan)的(De)使(Shi)用(Yong)寿(Shou)命(Ming)。(?)