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红外光度法测定水中矿物油的技术和应用
编辑 :

TIANJINSHINENGPUKEJIYOUXIANGONGSI

时间: 2017-07-21 浏览量: 5765

矿物油是由烷烃、环烷烃及芳香烃组成的混合物。早期的各种定量方法都是测量混合组分中部分化合物某一特性基团的特殊吸收(发射),进而推算混合组分总量;一旦具有该特性基团的化合物的相对含量发生变化,吸收系数必然相应变化,所以都存在“标准油”的选择问题,长期以来未能统一。新近颁布的GB/T 16488-1996首选了三波长红外光谱法作为统一方法,同时兼顾国情,保留了非分散红外法。本文对新国标的原理及实施中的一些技术问题进行了探讨。  

  1、 FEIFENSANHONGWAIFADEYUANLIJIJISHUJUXIANXING

悠洋棋牌  FEIFENSANHONGWAIFAYISHIYOULEIWUZHIDECH3、 CH2ZAI3.3~3.6 μm DETEZHENGXISHOUZUOWEICEDINGYOUHANLIANGDEJICHU。GAIFAZHILIYONGLEKUANGWUYOUZHONGCH3、 CH2LIANGGETEXINGJITUANDEHONGWAIXISHOUJINXINGCEDING,MEIYOUCANKAOQIZHONGFANGHUANDEXIANGYING,CUNZAI“YIPIANGAIQUAN”ZHIBUZU。WEIKAOCHAYINGYONGZHONGDEJUXIANXING,YONGBUTONGPEIBISHENZHIJIDUANBILIDEHUNHETINGJINXINGSHIYAN,JIEGUOJIANBIAO1。



No烃组成烷烃%(V)实测值mg/L回收率%
110:0:0100156142
27:3:0100137125
36.5:2.5:190136124
49:10:195123112
53:7:0100122111
69:2:191.7116105
75:3:188.9110100
84:2:185.710999.1
97:0:37010595.5
100:10:010010494.5
111:2:1758678.2
121:8:469.27971.8
130:7:3707870.9
143:0:7305247.3
150:3:7303632.7
160:0:100109.1


  BIAO1

悠洋棋牌  ZHU:TINGZUCHENGWEIZHENGSHILIUWAN:LAOJIAOWAN:JIABEN(V/V);XIAOZHUNYOUPEIZHIZHIWEI110mg/L(5:3:1V/V)

  由表1可见,非分散红外测油仪对标准油的依赖性确实太大,其所响应的只是烃组成中的CH3、 CH2。回收率对烷烃%(V)的相关性非常显著,P%=4.5+0.79*烷烃%(V),r=0.94;对芳环的响应则未给予应有的考虑,随着样品与校准油中芳烃含量差异的加大,误差也相应增大。

  2 、三波长红外光谱法

悠洋棋牌  2.1 SANBOZHANGHONGWAIGUANGPUFADEJISHULUXIAN

  矿物油是多种烃的混合物,烃类又存在同系物,无法获得各结构单元、组成比例完全一样的标样,没有常规定量方法的计量关系可以利用。ISO组织用“毋需标准样品的红外光谱定量法”-官能团分析法[1,2]推出了全新的红外分光光度法[3]。

悠洋棋牌  KUANGWUYOUCONGHUAXUEJIEGOUSHANGKANZHUYAOHANCH3、 CH2、FANGHUANSANZHONGJITUAN。QIZUCHENGZHONGDE“RENYIHUAHEWU”JUNKEYOUZHEISANZHONGJITUAN“PINZHUANG”ERCHENG,YINCIKEFENBIECEDINGKUANGWUYOUZHONGDESHANGSHUSANZHONGJITUANDELIANG,QUANBUJITUANLEIJIAHOUKEDEZONGLIANG。

  2.2 数学模型建立及其参数标定

悠洋棋牌  RONGYEZAIMOUYIBOSHUCHUDEXISHOUQIANGDUZHENGBIYUQIZHONGMOUZHONGJITUANDENONGDU,QIEXISHOUJUYOUJIAHEXING[2]。GEZHONGJITUANYOUBUTONGDEXISHOUQIANGDU,SUOYIJITUANLEIJIASHIYINGYIGELEIJITUANDEXIGUANGXISHUWEIQUAN,XIGUANGDUWEIQUANZHONG,JIAQUANLEIJI[2]。CH2、 CH3、FANGHUANDEC-HJIANSHENSUOZHENDONGXISHOUFENBIEZAI2930cm-1、2960 cm-1、3030cm-1CHU。YOUXISHOUDEJIAHEXINGKEZHI,SANBOSHUCHUDEXIGUANGDUA2930、A2960、A3030FENBIEWEISANLEIJITUANXISHOUDEFENLEIHUIZONGZHI,SUOYIQIYUANSHISHUXUEMOXINGWEI:

悠洋棋牌  C=x* A2930+y* A2960+z* A3030 (1)

悠洋棋牌  CWEIRONGJIZHONGKUANGWUYOUDENONGDU,x、y、z FENBIEWEICH2、 CH3、FANGHUANDEC-HJIANDEXIGUANGDUXISHU。YINZHITINGJIDUIFANGHUANDEXISHOUYOUDIEJIA,JINGUANHENXIAO,DANFANGHUANDEXIGUANGDUXISHUDA[2],YIYINQIDADEWUCHA,XUYINRUXIAOZHENGXISHUFDUIA3030XIUZHENG:

悠洋棋牌  C=x* A2930+y* A2960+ z*( A3030- A2930/F) (2)

  CIJI“SANBOZHANGHONGWAIGUANGPUFA”DEJIBENSHUXUEMOXING。


  LILUNSHANG,XISHOUXISHUWEITEDINGZHI,DANSUIYIQIJINGDU、CAOZUOTIAOJIANYOUCHABIE,KEJIEZHUMOXINGHUAHEWUDECHUNWUZHIBIAODINGBENYIQIDEZHI[4]。FENBIEPEIZHIFUHANCH2(RUZHENGSHILIUWAN)、 CH3(RULAOJIAOWANHUOYIXINWAN)、FANGHUAN(RUJIABENHUOBEN)JITUANDEDANYIBIAOZHUNRONGYEYIBIAODINGx,y,z:ZAI3400-1~2400cm-1ZHIJIANJINXINGHONGWAIGUANGPUSAOMIAO,MOXINGHUAHEWUDEHONGWAIGUANGPUJIANTU1。


TU1

悠洋棋牌  ZHUGELIANGQU3030 cm-1、2960 cm-1、2930 cm-1SANCHUDEXIGUANGDU,YICIDAIRU(2)SHI,DESANLIANFANGCHENGZU,QIZHONGFWEIZHENGSHILIUWANDEA2930/ A3030ZHI。

  DUIYITEDINGYIQI,ZAITEDINGTIAOJIANXIA,x、y、z、FBAOCHIWENDING,Nicolet 750ⅡHONGWAIGUANGPUYIDEXIANGYINGXISHUJIANBIAO2。

  2.3 系数验证及适应性检验

  WEIYANZHENGXIAOZHENGXISHU,FENBIEYONGGUOBIAOYANGJIZIPEIBZHONGYOUBIAOYANGJINXINGLEHUISHOULVSHIYAN,JIEGUOJIANBIAO3。

  BIAO2 Nicolet 750 Ⅱ HONGWAIGUANGPUYIDEXIANGYINGXISHU


光源溶剂xyzf
近红外CCL4114.19259.441582.582.5
中红外CCL4143.31199.2964.585.2
中红外TTE177.16230.651015.178.0


表3 国际样及B重油的测定结果


标样名称标准值(mg/L)测定值(mg/L)P%RE%
国际矿物油733010315.5±1.414.794.8-5
国际矿物油733040120.4±2.419.595.6-4
国际矿物油733010424.9±2.124.196.8-3
B重油10.09.9599.5-0.5%



悠洋棋牌  SHIYANJIEGUOBIAOMING,BENXIAOZHENGXISHUDEPINGJUNHUISHOULVWEI96.7%,XIANGDUIWUCHAZAI-0.5%~-5%ZHIJIAN,NENGMANZUSHIYONGCEDINGYAOQIU。

悠洋棋牌  SANBOZHANGHONGWAIGUANGPUFACHONGFENJIANGULELIANWAN、HUANWANJIFANGXIANGWANDEGONGTONGYINGXIANG,NENGSHIYINGGEZHONGZUCHENGBILIHUNHETINGDECEDING,BIKAILE“BIAOZHUNYOU”WENTI,JUYOUHENDADEYOUYUEXING。QIDUITINGZUCHENGBILIBIANHUADESHIYINGXINGYANZHENGJIANBIAO4。

  BIAO4BIAOMING,SANBOZHANGHONGWAIGUANGPUFADUIGEZHONGTINGLEIZUCHENGBILI,SHENZHIJIDUANBILIDEYANGPINJUNJUYOUHENHAODEXIANGYING,BUXUZAIMEICICEDINGYANGPINQIANTIQUHUOPEIZHI“BIAOZHUNYOU”,CHONGFENXIANSHICHUGAIFADUIYANGPINZHONGTINGLEIZUCHENGBIANHUASUOTEYOUDESHIYINGXING。

悠洋棋牌BIAO4 TINGZUCHENGBIANHUADUISANBOZHANGFADEYINGXIANG(PEIZHIZHI105mg/L)


烃组成9:2:14:2:11:2:41:8:49:10:110:0:00:10:00:0:10
实测值mg/L113.4111.6104.9113.2115.2110.7109.499.3
回收率%108106.399.9107.8109.7105.4104.294.6
芳烃%(V)8.314.357.130.8500100


悠洋棋牌  ZHU:TINGZUCHENGWEIZHENGSHILIUWAN:LAOJIAOWAN:JIABEN(V/V).

悠洋棋牌  3 、WENTITAOLUNJIJISHUYINGYONG

  3.1 WENTITAOLUN

悠洋棋牌  FEIFENSANFAYINBUJUFENGUANGGONGNENG,WUFAFENBIECELIANGGEJITUANDEXISHOUQIANGDU,ZHINENGJIANDANJIAHE,BUDANYANGPINYUBIAOZHUNYOUZHONGFANGTINGHANLIANGDECHAYIHUIYINQIDADEWUCHA,SHENZHIYUYANGPINYUXIAOZHUNYOUZHONGCH3YUCH2BILIDEGAIBIANYEHUIYINQIBUXIAODEWUCHA,RUBIAO1ZHONG,1#←→10#,2#←→5#,9#←→13#,14#←→15#SHIYAN,TONGYANGDEWANTINGHANLIANG,JIEGUOQUECHAYIBUGOU(YINρZHENGSHILIUWAN:ρLAOJIAOWAN≈1,TINGZUCHENGZHONGZHENGSHILIUWANYULAOJIAOWANDETIJIBIJINSIWEIZHONGLIANGBI)。

  JIN、ZHONGHONGWAIQUSUIWUYANGEJIEXIAN,DANFEIFENSANYISHIYONGJINHONGWAIGUANGYUAN,CELIANGZHONGHONGWAIQUDEXINXI(JINHONGWAIGUANGQUBIANYUAN),NENGLIANGRUO、LINGMINDUDI,YOUQISHIDUIFANGHUANDEXIANGYING(DAXINGYIQIYIRUCI,JIANBIAO2)。JIANYIGUOCHANSANBOZHANGYOUCEDINGYISHIYONGZHONGHONGWAIGUANGYUAN,YIJINYIBUTIGAOYIQILINGMINDU。

  SANBOZHANGHONGWAIFAFEIYANGEANHUAXUEJILIANGGUANXIJINXINGCEDING,LILUNSHANG,CELIANGFEIJUEDUIZHUNQUE,RUHULVELEKUANGWUYOUZHONGDECIJIAJI。CIJIAJIYINXISHOUJIRUO,BUYIJIANCHU[2],YEZHAOBUDAOHUAXUEMOXINGHUAHEWUBIAODINGQIXISHOUXISHU。DANQIZAITINGHUAHEWUFENZIZHONGSUOZHANBILIHENXIAO,SUOYINQIDEWUCHADUIZONGTILAISHUOYINGXIANGBUDA,GUKEYISHENGLVE。

  SHIJIYINGYONGZHONG,FUZAYANGPINDEXISHOUWANGWANGFASHENGYIDINGDEHONGYIHUOLANYI,SUOXUANBOZHANGBUKENENGBAOZHENGZAIZUFENDEFENGZHIXISHOUCHU[2],RUFANGHUANDEXISHOUBOSHUCHANGZAI3030~3070cm-1[2]JIAN。SUOYI,XIGUANGDUDELIANGQUBUYINGJIXIEDINGWEIMOUYIBOSHUDIAN,ERYINGRENWEIGAIBOSHUCHUXIANGYINGDEXISHOUFENG,BURANXIGUANGDUQUYUFENGYAO,SHENZHIYUFENGJIAO,DOUHUIYINQIYINQICEDINGJIEGUODEPUBIANPIANDI。ZHUANYONGCEYOUYIDUIPUTUDECHULISHIYI“HEIXIAZI”,CHENGXUSHEJISHIGENGYINGZHUYIGAIWENTI。

悠洋棋牌  YOUTIAOJIANKEKAOLVYONGJIFENXIGUANGDUFA[2]DAITIXISHOUFENGGAOFADINGLIANG,JIKETIGAOCEDINGJINGDU,YEKEYOUXIAOFANGZHIXIGUANGDUQUZHIBUDAOWEI。

GUANGDUFENXIZAIA=0.3≈0.6FANWEINEIWUCHAJIAOXIAO,YOULIANGXIGUANGDUWEI0.43[4]。FANGHUANZHONGC-HJIANDEGANDUYUANXIAOYUCH3、CH2,QIXISHOUXISHUZDEZHUNQUEYUFOUDUICEDINGJIEGUOYINGXIANGXIANZHU;F=A2930(ZHENGSHILIUWAN)/A3030(ZHENGSHILIUWAN),ZHENGSHILIUWANBUHANFANGHUAN,A3030HENWEIRUO,TAIXIAODEA3030YIJIFJISUANDAILAIHENDADEWUCHA。YINCI,ZAIBIAODINGX、Y、Z、FXISHUSHIBUBIJUNIYUGUOBIAOZHONGSUOGUIDINGDENONGDU;YINGSHIYIQIXIANGYINGQINGKUANGSHIDANGDIAOZHENGMOXINGHUAHEWUDENONGDU,BAOCHIAZAIHESHIXISHOUFANWEI,YIHUOQUZHUNQUEDEYIQIXISHU;MOXINGHUAHEWUDENONGDUZHIGONGJIELIANLIFANGCHENGZUYONG,QIZHIYEBUBICOUZHENG,YINGYIPEIZHIZHUNQUEWEIZHONG(3.2.1.3)。

  3.2 技术应用

  3.2.1 YINGYONGZHONGJIGEGUANJIANXINGWENTI

悠洋棋牌  3.2.1.1 RONGJIDEXUANQU

悠洋棋牌  CCL4SHIGAODUXINGRONGJI,TTEDIDU、FUSHIXINGXIAO,DANGUANGXUEXINGNENGJIDUIYOUDETIQUNENGLI(ZHINENGRONGJIEQINGYOUHEBUFENZHONGYOU)DOUBURUCCL4。YINGGENJUCEDINGYAOQIUJIBEICEDUIXIANGZHENDUIXINGXUANZE。

悠洋棋牌  3.2.1.2 FANGFADEXUANYONG

  YOULEIWUZHIZHONGSUOHANDEFANGTINGSUIJIAOWANTINGSHAODEDUO,DANQIDUXINGHESHUIRONGXINGQUEDADEDUO;FANGHUANDEGANDUBICH3、CH2XIAOYIGESHULIANGJI,DUICEDINGJIEGUODEYINGXIANGJIAODA,YINCIDUIFANGHUANDEZHUNQUEXIANGYINGYOUWEIZHONGYAO。FEIFENSANHONGWAIYIYINBUJUFENGUANGNENGLI,WUFAJIAQUANLEIJI,SHEQILEFANGHUANXINXI,SHIYONGSHIYINGJIAYIZHUYI。


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