188体育

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超高强度钢中的Al,Mn,Si,Ti测定(二)

发布时间:2015-05-20 00:00 作者:北纳创联
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2JIEGUOYUTAOLUN

2. 1RONGJIEXINGSHIYAN

ICP CELIANGGANGZHONGYUANSUDERONGJIEFANGFAZHUYAOSHIYILIULINHUNSUANMAOYAN – DIJIAXIAOSUANQUCHUTANHUAWUDEXINGSHIWEIZHU, DANSHIJINGMAOYANCHULIHOUDERONGYEYIYINRUWURAN, DUIHENLIANGYUANSUCELIANGZAOCHENGKUNNAN。DUI 0.5 g DEYANGPINJINXINGRONGJIESHIYAN, JIEGUOJIANBIAO 1。

YOUBIAO1KEYIKANCHU,YONGYANSUAN、XIAOSUANRONGJIEYANGPIN,DANGJIARUYANSUAN5mL HOU,YANGPINYIJINGRONGJIE,DANJIARUGUOLIANGDEYANSUAN,BINGBUNENGSHIYANGPINZHONGYOUHEISEZHANFUWURONGJIE;JIARUQINGFUSUANRONGJIESHIYANG,NENGSHIRONGJIESUDUJIAKUAI, DANHEISEZHANFUWUYIRANCUNZAI;30DI(YUE3mL) QINGFUSUANYEMEIYOURONGJIEHEISEZHANFUWU,ZHEIBIAOMINGCIWUZHISHIYOULITAN。YONGLIUSUANMAOYANCHULIHEISEZHANFUWURONGYE,RONGYECHENGQING,YINCIKEJINYIBUQUERENWEITAN。YOULITANBURONGJIEYUWANGSHUIHEQINGFUSUANZHONG, YINCIWULUNJIADUOSHAOSUAN,JUNBUNENGSHIYANGPINRONGJIECHENGQING。JIARULIUSUANHOURONGYECHENGQING,DANMAOYANDECHULIFANGFAHUISHISiYUANSUSUNSHIERWUFACELIANG。JINGGUOSHIYANDUIZHAO, YOULITANDECUNZAIBUHUIDUIDAICEYUANSUDECEDINGCHANSHENGYINGXIANG。YOUBIAO1KEZHI,BIANHAO1~3 DERONGYANGFANGFAKEYIHENHAODIRONGJIEYANGPIN, XIANXIANGYUYONGQINGFUSUANRONGJIEDEYANGPINYIZHI,YINWEISUOYANJIUDECAILIAOHANGUILIANGJIAODI,YONGYANXIAOSUANRONGJIESHIYANGNENGGOUMANZUKETIYAOQIU, ZUIZHONGXUANZEYONGYANSUAN15 mL、XIAOSUAN3mLRONGJIESHIYANG。

2. 2FENXIXIANDEXUANZE

GAOQIANGDUGANGZHONGJITIJIGONGCUNYUANSUYOU Fe, Ni, Co,Mo, Cr, Mn, Si, Ti, Al, V, W, Nb DENGYUANSU。ZHEIXIEYUANSUHANLIANGFANWEIBUTONG, DUIFENXIYUANSUDEGUANGPUGANRAOJINXINGYANJIU, YOULIYUXUANZEWUGANRAOHUOGANRAOZUIXIAODEPUXIANJINXINGCELIANG。BENSHIYANCAIYONGDE ULTIMA FASHEGUANGPUYIDEGUANGZHAKEDUWEI4320 TIAO/mm, FENBIANLVJIAOGAO, KEYIHENHAODIBIMIANGUANGPUGANRAO。

PEIZHICHENGRUBIAO 2( AN 0.500 0 g YANGPINDINGRONGZHI 50 mLJISUAN ) SUOSHIDEDANYIYUANSUCESHIRONGYE, ZAIGEFENXIYUANSUDE2~3 TIAOFENXIPUXIAN ( JUTIYUXUANFENXIXIANJIANBIAO 3) ZHONGXINBOZHANGFUJINDE 0.184 2 nm CHUANGKOUFANWEINEIJINXINGSAOMIAO, HUODEDANYIGANRAOYUANSURONGYE、 FENXIYUANSURONGYEJISHIJIKONGBAIRONGYEDEGUANGPUSAOMIAOTUXING, DUIPUTUJINXINGDIEJIA、 FANGDACHULI, YANJIUQIGUANGPUGANRAOQINGKUANG。

2.2.1LVDEFENXIXIANXUANZE

TONGGUOPUTUGUANCHA, Co, Cr, Fe YUANSUDUI Al 237.312FENXIPUXIANYOUGANRAO; ZAI Al 392.152 nm FENXIXIANZHONGYANG,Mo YUANSUYOUXIANGTONGDEPUXIANCUNZAI, LIANGTIAOPUXIANJIHUZHONGDIE, CUNZAIYANZHONGDEPUXIANZHONGDIEGANRAO; ZAI Al 309.271 nm FENXIXIANZHONGYANG, Nb YUANSUYOUXIANGTONGDEPUXIANCUNZAI, LIANGTIAOPUXIANJIHUZHONGDIE, CUNZAIYANZHONGDEPUXIANZHONGDIEGANRAO; SUOYOUGONGCUNYUANSUJUNDUIAl 394.401 nm PUXIANWUMINGXIANGANRAO。YINCIXUAN Al 394.401nm ZUOWEIFENXIPUXIAN。

2.2.2MENGDEFENXIXIANXUANZE

通过谱图观察,Cr,Fe,Mo,W元 素 对Mn280.106 nm 分析谱线均有光谱干扰存在, 其它元素对此谱线无干扰; Cr, Mo 元素在 Mn 293.306 nm 分
析谱线的两侧有峰存在, 其它元素对此谱线无干扰;Mo 293.219 nm 和 Mo 293.430 nm 谱线存在两条谱线的尾翼均未延伸至谱线的中央, 不存在谱线重叠干扰, 但有背景干扰存在; 对于 Mn 257.610 nm 分析线, Fe 元素对此分析谱线左右两侧有光谱干扰存在, 其它元素对此谱线无干扰。综上所述, 共存元素对 Mn 257.610 nm 谱线均无谱线重叠干扰, 但在 Mn257.610 nm 处, Fe 元素的强度值与空白值相比稍微偏高, 由于无谱线重叠干扰, 可认定为背景干扰。其它两条谱线均存在干扰谱线, 因此选 Mn 257.610nm 谱线作为分析线。

2.2.3GUIDEFENXIXIANXUANZE

GUIYUANSUSHIZIRANJIEZHONGPUBIANCUNZAIDEYUANSU, YINCIZAISAOMIAOTUZHONG, GUIYUANSUDEPUXIANPUBIANCUNZAIQIEZAITONGYIQIANGDU, ZHEIZHONGGANRAODUICELIANGMEIYOUYINGXIANG, ZAISHIJIGONGZUOZHONGKEYITONGGUOSHIJIYIZHIXINGKOUCHU。TONGGUOPUTUGUANCHA, Fe YUANSUZAI Si 251.611nm FENXIPUXIANDELIANGCEYOUFENGCUNZAI, QITAYUANSUDUICIPUXIANWUGANRAO; Nb, W, Cr, Co, Fe, Mo YUANSUZAI Si 251.921 nmFENXIPUXIANDELIANGCEYOUFENGCUNZAI, QITAYUANSUDUICIPUXIANWUGANRAO; GONGCUN Nb YUANSUDUI Si 251.921 nm DEPUXIANCUNZAIGUANGPUGANRAO, LIANGGEYUANSUDEFENGJIHUZHONGDIE, CUNZAIYANZHONGDEPUXIANZHONGDIEGANRAO; Cr, Mo YUANSUZAI Si 288.158 nm FENXIPUXIANDELIANGCEYOUFENGCUNZAI, QITAYUANSUDUICIPUXIANWUGANRAO。ZONGSHANGSUOSHU,GONGCUNYUANSUDUI Si 251.611 nm WUPUXIANZHONGDIEGANRAO, DAN FeYUANSUZAIFENXIXIANCHUYOUYIRUOFENGCHUXIAN, GAIFENGWEISHIJIHESHUIJICHUNTIEZHONGJIAZADE Si YUANSU, CIXIANXIANGKEYITONGGUOSHIJIPIPEIHESHIYONGCHUNDUGENGGAODECHUN Fe JIAYIXIAOCHU, QIYUYUANSUJUNYOUGANRAOYUANSUCUNZAI。YINCIXUANZE Si 251.611 nm PUXIANZUOWEIZUIZHONGFENXIXIAN。

2.2.4 TAIDEFENXIXIANXUANZE

TONGGUOPUTUGUANCHA, Cr, Fe YUANSUZAI Ti 323.904 nm FENXIPUXIANDELIANGCEYOUFENGCUNZAI, QITAYUANSUDUICIPUXIANWUGANRAO;Fe YUANSUZAI Ti 338.376 nm FENXIPUXIANDELIANGCEYOUFENGCUNZAI,QITAYUANSUDUICIPUXIANWUGANRAO; Ti 334.941 nm FENXIXIANDEZUOCEYOULINGYIGEQIANGDUJIAORUODE Ti YUANSUFENXIPUXIANCUNZAI, DANLIANGTIAOFENXIPUXIANMEIYOUJIAOCHAZHONGDIE, KEYIDULIFENXI, BUCUNZAIPUXIANZHONGDIEGANRAO, 334.941 nm PUXIANQIANGDUJIAODA, SHIHECELIANGDIHANLIANG, YINCICAIYONGGAIFENXIXIANZUOWEIZUIZHONGFENXIXIAN。

ZONGHESHANGSHUPUTUGANRAOQINGKUANG, GEYUANSUDEZUIZHONGCELIANGPUXIANWEI Al 394.401 nm, Mn 257.610 nm, Si 251.611nm, Ti 334.941 nm。

2. 3XIANXINGFANGCHENGYUJIANCHUXIAN

ZAIQUEDINGDETIAOJIANXIAANZHAOYIQIJISUANJISHEDINGDECHENGXU,DUIXILIEBIAOZHUNSHIYONGRONGYEYICICELIANG, YIZHILIANGNONGDU x WEIHENGZUOBIAO、 XINHAOQIANGDU y WEIZONGZUOBIAOJIANLIGONGZUOQUXIAN。DUIKONGBAIYANGPINJINXINGPINGXING 12 CIFENXI, JISUANCEDINGJIEGUODEBIAOZHUNPIANCHA。GENJUGONGSHI (1) JISUANFENXIFANGFACEDINGMOUDAICEZUFENDEJIANCHUXIAN。XIANXINGFANGCHENG、 XIANXINGFANWEI、 XIANGGUANXISHUJIFANGFAJIANCHUXIANJIEGUOJIANBIAO 4。

cL=kSb/b(1)

式中: c L ——待测组分的检出限, mg/L ;

S b ——测量空白样品的标准偏差, mg/L ;

b——DINONGDUQUXIAOZHENGQUXIANDEXIELV, TABIAOSHIDAICEZUFENGAIBIANYIGEDANWEISHI, FENXIXINHAODEGAIBIANLIANG, JILINGMINDU;

k——与置信度有关的常数, IUPAC 建议 k=3.95%。

2. 4JINGMIDUHEZHUNQUEDUSHIYAN

GENJUYANGPINFENXIFANWEI (Al 0.004%~0.10% ; Mn 0.01%~0.05% ; Si 0.01%~0.05% ; Ti 0.01%~0.05%)

XUANZEXIANGYINGDEBIAOZHUNYANGPIN, JINXINGLEJINGMIDU、 ZHUNQUEDUSHIYAN,JIEGUOJIANBIAO 5 JIBIAO 6。

YOUBIAO 5 KEZHI, Al, Mn, Si, Ti YUANSUCEDINGJIEGUODEXIANGDUIBIAOZHUNPIANCHAXIAOYU10%, SHUOMINGFANGFAJUYOULIANGHAODEJINGMIDU。

YOUBIAO 6 KEZHI, YANGPINJIABIAOHUISHOULVZAI 94%~120% ZHIJIAN, SHUOMINGGAIFANGFAJUYOUJIAOGAODEZHUNQUEDU, KEYIYONGYUCHAOGAOQIANGDUGANGZHONG Al, Ti, Si, Mn HANLIANGCEDING。

3JIEYU

CAIYONG ICP–AES FACEDINGCHAOGAOQIANGDUGANGZHONGDE Al,Mn, Si, Ti HANLIANG, TONGGUOGUANGPUGANRAOSHIYANQUEDINGZUIJIAFENXIXIAN, GAIFANGFACELIANGZHUNQUEDUHEJINGMIDUJIAOGAO, NENGMANZURICHANGCESHIXUYAO。

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