□ 王乐新 王云
KAER·FEIXIUKULUNFAWEILIANGSHUIFENCEDINGYIGUANGFANYINGYONGYUCEDINGSHIYOU、HUAGONG、QINGGONG、DIANLI、YIYAO、NONGYAO、HUANBAO、DIZHI、SHIPINDENGXINGYECHANPINZHONGDESHUIFENHANLIANG。YOUYUJINNIANGEDANWEIDUICHANPINZHILIANGDEZHONGSHI,DUIGAIZHONGYIQIDEYINGYONGZHUNIANZENGJIA,YINCIZHIDINGGAIZHONGYIQIDEJIANDINGGUICHENGJIUXIANDEYOUWEIPOQIEHEZHONGYAO。JINGGUONULI,JJG1044-2008《KAER·FEIXIUKULUNFAWEILIANGSHUIFENCEDINGYI》JIANDINGGUICHENGYU2008NIAN9YUE27RIJINGGUOJIAZHIJIANZONGJUPIZHUNFABU,BINGZI2009NIAN1YUE1RIQISHIXING。
GUICHENGFABUSHISHIHOU,QUANGUODEZIXUNDIANHUABUSHAO。YOUYUGAIZHONGYIQICAOZUOJIAOWEIJIANDAN,GUICHENGZHONGDEJIANDINGFANGFABIJIAOXIANGXI,YINCIZIXUNYIQIJIANDINGFANGFADEJIAOSHAO, ERZIXUNBIAOZHUNWUZHIXIANGGUANWENTIDEJIAODUO。ZAIXIEGAIGUICHENGSHI,YIQICEDINGDIHANSHUILIANGZHIDEJIANDING,XUYAOYOUGUOJIABIAOZHUNWUZHIDEZHICHENG,DANGSHIGUOJIAJILIANGYUANYIYOUSHUI-JIACHUNBIAOZHUNWUZHI,SHUIHANLIANGWEI1mg/g,DANSHIYOUYUSHENGCHANLIANGHENSHAO,JINGCHANGMAIBUDAO。WODANWEIXIANZAIZHENGZAIYANZHIHESHENBAOSHUI-JIACHUNBIAOZHUNWUZHI, DANZHEIXUYAOYIGEBIJIAOZHANGDEGUOCHENG。BIAOZHUNSHUIRONGYEMAIBUDAO,DANJIANDINGSHUIFENCEDINGYIYOUBIXUYOUSHUI-JIACHUNBIAOZHUNRONGYECAIXING,ZENMEBAN? MUQIANZHUANGKUANGXIA,ZHINENGZIJIPEIZHI。ZAIKONGZHIHAOBUQUEDINGDUDEQIANTIXIA,SHIKEYIZIJIPEIZHISHUI-JIACHUNBIAOZHUNRONGYEDE。XIAMIANJIUGUICHENGQICAOZHONGSUOYUDAODEYIXIEWENTIHEXIANGFA、GUICHENGDESHIYONGFANWEI、ZAIYIQIJIANDINGZHONGDEZHUYISHIXIANGHEBIAOZHUNWUZHIDEPEIZHIFANGFADENGZUORUXIASHUOMING。
一、关于规程的名称及适用范围的说明
GUANYUGUICHENGDEMINGCHENG,WEISHENMEBUCHENGZHIWEI《WEILIANGSHUIFENCEDINGYI》JIANDINGGUICHENG, ERBIXUXIANDINGZAIKAER·FEIXIUKULUNFAWEILIANGSHUIFENCEDINGYIDEFANWEI?JULEJIE,WEILIANGSHUIFENCEDINGYIDEZHONGLEIMUQIANANFENXIFANGFADAZHIFENWEIHONGGANFASHUIFENCEDINGYI、DIANZU(DIANDAO)FASHUIFENCEDINGYI、KAER·FEIXIUTIJI(DIDING)FASHUIFENCEDINGYI、KAER·FEIXIUKULUNFASHUIFENCEDINGYISIDALEI。QIANLIANGZHONGYIYOUGUOJIAJILIANGJIANDINGGUICHENG,CICIBIANXIEGUICHENGKAISHIXIANGBAKASHITIJI(DIDING)FAHEKASHIKULUNFADOUXIERUGUICHENG,DANHOULAIFAXIANKASHIDIDINGFADEYIQIZHONGLEIJIAODUO,JISHUZHIBIAOCHABIEYOUTAIDA,ZHIYOUJINKOUDESHUZIDIDINGSHIYIQIHEKULUNFAYIQIJISHUZHIBIAOJIEJIN。BIZHEZAIDUONIANDEYIQIJIANXIAOGUOCHENGZHONGFAXIAN,GUOCHANSHUZITIJI(DIDING)SHISHUIFENYIYOUYUJINGMIJIAGONGJISHUJIAOCHA,HUOSHICAILIAONAIMOXINGJIAOCHADENGYUANYIN,YIQICHUCHANGSHIJISHUZHIBIAOHAIKEYI,DANSHIYONGJINIANHOU,YOUYUMOSUN、MIFENGJISHUJIAOCHAHUOJIXIECHUANDONGHUICHAJIAODA,JISHUZHIBIAOXIAJIANGHENDUO,BATAMENXIANDINGZAIYIGEGUICHENGZHONG,JIANGHUIZAOCHENGHENDUOYIQIBUHEGE。CIWAI,KASHISHOUDONGTIJI(DIDING)SHISHUIFENCEDINGYICELIANGFANWEIZHAI、ZHUNQUEDUDI,RUOYAOTUOKUANCELIANGFANWEI、TIGAOZHUNQUEDU,ZHENDUIBUTONGDEJIANDINGJIUBIXUPEIZHIBUTONGDIDINGDUDEDIDINGYEDUOZHONG,DANDUIDIDINGYEDEBUQUEDINGDUJINXINGFENXIYOUCHENGWENTI, BINGQIEDIDINGYEBUYICUNFANG,DIDINGDURONGYIGAIBIAN。SUOYI,ZUIHOUMEIYOUBA“TIJI(DIDING)SHIWEILIANGSHUIFENCEDINGYI”XIERUGUICHENGZHONG。ER“SHUZITIJI(DIDING)SHIWEILIANGSHUIFENCEDINGYI”KEYICANZHAOBENGUICHENGZHIXING(JISHUZHIBIAOXIANGJIN)。
二、规程的试验情况
ZAIGUICHENGQICAOGUOCHENGZHONG, WOMENTONGGUOHESHENGCHANCHANGJIAHEZUODEFANGSHI, DUIKAER·FEIXIUKULUNFAWEILIANGSHUIFENCEDINGYIJINXINGLEDALIANGDESHIJIJIANCE,WEIBIANXIEGUICHENGJILEILEDIYISHOUJISHUSHUJU。WEILIANGSHUIFENCEDINGYIDEXIAOZHUNGONGZUOZAIWOYUANYIKAIZHANDUONIAN,GUOQUWOMENZAISHUIFENYIDEJIANCEZHONG,DADUOCAIYONGXIANGDUISHIZHIWUCHAFANGSHI。ZAIGUICHENGBIANXIECHUQIYEXIANGCAIYONGXIANGDUISHIZHIWUCHADECELIANGFANGSHI,DANWOYUANXIAOZHUNGUIFANYAOQIUXIAOZHUNDESHUIFENHANLIANGJIAODA,ZAI(500~5000)μgFANWEINEI,YONGCHUNSHUICELIANGYIQIDEXIANGDUISHIZHIWUCHASHIKEXINGDE。DANSHISHUIFENZAI500μgYIXIAFANWEIDECELIANG,ZAISHIJIYINGYONGZHONGSHIZUIDUODE,ZHEIGEFANWEINEIDEZHUNQUEYUFOUSHIFEICHANGZHONGYAODE,ZHEIYESHIBIANXIEGUOJIAJILIANGJIANDINGGUICHENGDEZHUYAOMUDE。YINCI,GUICHENGZHONGBIXUBAOHANJIWEILIANGSHUIFENDUAN。DANGSHUIFENWEI10μg
SHI,ZAIJINCHUNSHUIYIJINGBUXINGLE,JISHIJINSHUI-JIACHUNBIAOZHUNRONGYE,QIYIQIDEXIANGDUISHIZHIWUCHAYETAIDA,DADAO30%YISHANG,WOMENBASHIZHIWUCHA30%YISHANGDEYIQIPANDINGWEIHEGEXIANRANSHIBUHESHIDE。NEIME,SHIFOUKEJIANG10μgDIANDINGWEIJUEDUIWUCHA,QITAJIANDINGDIANDINGWEIXIANGDUIWUCHA? SHIZHIWUCHAPINGDINGBIAOZHUNJIBUTONGYI,BUQUEDINGDUFENXIYOUBUHAOPINGDING,ZUIHOUHAISHIJIANGSHIZHIWUCHATONGYICAIYONG±(5%JIANDINGDIAN+3)μgLAIPINGDING, ZHEIYEFUHEYIQICELIANGFANWEINEIDEWUCHAXIANXINGFENBUTEXING。
三、测量为何不取范围而取检定点
ZAIQITAGUICHENGZHONGDADUOQUJIANDINGCELIANGFANWEIERBUSHIJIANDINGDIAN。QIEQUCELIANGFANWEIDEGUICHENG,JIANDINGYONGBIAOZHUNWUZHIDEHANLIANGDADUOSHIBULIANXUDE,ERSHUIFENCEDINGYIDESHUIHANLIANGJIANDINGYONGBIAOZHUNWUZHISHILIANXUDE。ZHEIJIURONGYIDUITONGYITAIYIQIDAILAIBUTONGDEPINGJIAJIEGUO。BIRUYOUYITAIZAI10μgDIANBUHEGE,DANZAI100μgDIANQUEHEGEDEYIQI,DANGBASHIZHIWUCHADINGWEI(10~100)μgCESHUIFANWEISHI,JINYANGJIEJIN10μgDIANSHIPANDINGYIQIWEIBUHEGE;DANGJINYANGJIEJIN100μgDIANSHIPANDINGYIQIWEIHEGE,TONGYIFANWEI,TONGYITAIYIQIQUEYOUYUCELIANGFANGSHIBUTONGYIERDAILAIBUTONGDEPINGJIAJIEGUO,BUHAOJIEDING。XUANZEJIANDINGDIANWUCHAJIUCHANSHENGZAIZHEIGEDIANSHANG,ZHEIYANGJIAOKEXUE,BUHUIYINCELIANGFANGFABUTONGERDAOZHIYIQIHEGEHUOBUHEGEDEBUTONGJIEGUO,YINCI,ZUIHOUHAISHIQUEDINGYONGJIANDINGDIANLAIJIANDINGYIQIDESHIZHIWUCHA。
四、标准物质为何选取甲醇-水
SUIYOUXUDUOSHUIHANLIANGBIAOZHUNWUZHI, DANJJG1044-2008CAIYONGSHUI-JIACHUNBIAOZHUNWUZHIZUOWEIJIANDINGYONGBIAOZHUNWUZHI。WEIHEBUCAIQUQITAGUTIBIAOWUHEYETIBIAOWUNI? ZHUYAOYUANYINSHIGUTIWUZHIQUYANG、CHENGYANG、JINYANGGUOCHENGJIAOZHANG,BAOLUZAIKONGQIZHONGYIGAIBIANSHUIFENHANLIANG,JINYANGSHIHAIXUDAKAIDIANJIECHI,ZHISHIDIANJIECHIZHONGJINRUHANSHUIDEKONGQIERYINGXIANGCELIANGJIEGUO,QITARONGYEBIAOWUYOUYUNEIHANWUCHENGFENBUTONGKENENGYUDIANJIEYEFASHENGFANYING,ERSHUI-JIACHUNBIAOZHUNWUZHIZHONG,JIACHUNSHIDIANJIEYEDEZUCHENGBUFEN,SHUISHIBEICEBIAOWU,YOUYUCEDASHUILIANGZHISHIZHIJIEJINCHUNSHUI,ZHIYOUZAIWEISHUILIANGZHISHICAIJINSHUI-JIACHUNBIAOZHUNWUZHI,ZHEIYANGBIAOZHUNWUZHIBUZHIYUYINGXIANGDIANJIEYEDEPEIBIJILINGPINGHENGDIAN。SUOYI,CAIYONGSHUI-JIACHUNBIAOZHUNWUZHI。
五、检定项目的设立及意义
1.SHIZHIWUCHA:JIANDINGYIQISHUIHANLIANGCELIANGJIEGUOSHIFOUZHUNQUE。
2.CELIANGZHONGFUXING:JIANDINGYIQIZAICELIANGXIANGTONGSHUIHANLIANGWUZHISHIDEZAIXIANXING。
3.DIANJIESUDU:JIANDINGYIQIDEFENXIXIAOLV。
4.LINGDIANPINGHENGSHIJIAN:JIANDINGYIQIMIFENGSHIFOUWANHAO、DIANJISHIFOUWURAN、DIANJIEYESHIFOUGUOQI、FANGDADIANLUSHIFOUWENDINGDENG。
5.JUEYUANDIANZU:JIANDINGYIQIDEANQUANXINGNENG。
6.JUEYUANQIANGDU:JIANDINGYIQIDEANQUANXINGNENG。
7.XIELOUDIANLIU:JIANDINGYIQIDEANQUANXINGNENG。
六、检定中应注意的事项
WOMENZAIRICHANGJIANDINGZHONGFAXIAN,YONGCHENGZHONGJINYANGFAJIANDINGYIQIBIYONGTIJIJINYANGFACELIANGWUCHAYAOXIAO,DANJIAOWEIMAFAN。RUGUOJIANDINGYIQIHETIANPINGSHIJIAOJINHAIKEYI,DANRUGUOJIAOYUAN,JIANDINGJIUJIBUFANGBIAN。ERYONGTIJIJINYANGFAJIANDINGYIQIZAIDABUFENQINGKUANGXIASHIKEXINGDE(JINYANGQIWUCHAJIAODASHI、RENWEIJINYANGWUCHAJIAODASHIZEBUXING),DANGYIQIYONGTIJIJINYANGFAJIANDINGWEIHEGESHI,KEYIPANWEIHEGE。DANGYIQIJIANDINGWEIBUHEGESHI,ZAIJIANGYIQIBANDAOTIANPINGSHIFUJINJINXINGCHENGZHONGJINYANGLAIZUIZHONGPANDINGYIQISHIFOUHEGE。CIWAI,GUICHENGZHONGYOUYICHULURUXINGCUOWU,JIDIANJIESUDUDEJILIANGXINGNENGYAOQIUYINGWEI10min,YUGUICHENGFULUCHEDZHONGDEDIANJIESUDUDEJISHUYAOQIUXIANGYIZHI。
七、水-甲醇标准溶液的配制
RUHEPEIZHISHUI-JIACHUNBIAOZHUNRONGYE? XIEGUICHENGSHI,WEILEKAOXIANGYIYOUDESHUIBIAOZHUNWUZHI, ERCAIYONGDE1mg/gSHUI-JIACHUNBIAOZHUNWUZHI,1mg/gSHUIBIAOZHUNWUZHINENGYONG, DANBINGBUSHIJIANDINGSHUIFENCEDINGYIDEZUIJIAPEIBI,YINSHUIHANLIANGTAIDIJIYIXISHOUKONGQIZHONGDESHUIFEN,ERYINGXIANGCELIANGJIEGUO。ZUIJIAPEIBIWEI10mg/mL(HUO10mg/g)ZUOYOU。XIANDUIPEIZHIFANGFAJIZHUYISHIXIANGZUOJIAOWEIXIANGXIDESHUOMING。SUOXUSHEBEI:TIANPING:SHIWANFENZHIYI;TIJIDIDINGFASHUIFENCEDINGYI:JIANCEHEGE;JIACHUN:SEPUCHUN(YEXIANGSEPUYIYONGJIKE,ZUIHAOSHIXINDE,HANSHUILIANGDI);RONGLIANGPING:AJIHEGE;WEILIANGJINYANGQI:JIANCEHEGE。
(1)SHOUXIANBIXUPEIZHIJIAODADELIANG,YINWEIJIACHUNYIXISHUI,JIACHUNLIANGSHAOXISHOUKONGQIZHONGDESHUIFENZHANBIJIAODA;BENDICELIANGSHISHUIFENHANLIANGBIANHUAJIAODA; CHENGLIANGTIANJIASHUIFENWUCHAJIAODA。RONGLIANGPINGZHISHAOYINGZAI100mLYISHANG。
(2)XUANQUSEPUCHUNJIACHUN,DAORUYIZHIZHONGLIANGDERONGLIANGPINGZHONG,YAOYUN。CHOUQU500μLZUOYOUJIACHUNCHENGZHONGHOUJINYANGDAOYIPINGHENGHAODETIJIDIDINGFASHUIFENCEDINGYIZHONG,ZAICHENGZHONG。LIANXUJINYANG6CI,SUANCHUJIACHUNZHONGDEBENDIHANSHUILIANG,CHENGLIANGZHUANGJIACHUNDERONGLIANGPINGZHONGLIANG,SUANCHUJIACHUNLIANG,ZAISUANCHUYINGTIANJIADECHUNSHUILIANG,YONGSHIYIDEJINYANGQICHOUSHUIZAITIANPINGCHENGLIANGHOUTIANJIA,DEDAO10mg/gDESHUI-JIACHUNRONGYE。
(3)XUANQUSEPUCHUNJIACHUN,DAORURONGLIANGPINGZHONG,YAOYUN。CHOUQU500μLZUOYOUJIACHUNCHENGZHONGHOUJINYANGDAOYIPINGHENGHAODETIJIDIDINGFASHUIFENCEDINGYIZHONG,ZAICHENGZHONG。LIANXUJINYANG6CI,SUANCHUJIACHUNZHONGDEBENDIHANSHUILIANG,ZAISUANCHUYINGTIANJIADECHUNSHUILIANG, JIANGCHUNSHUIZHURUZHUANGJIACHUNDERONGLIANGPINGZHONG,ZAIZHURUJIACHUNZHIKEXIAN,DEDAO10mg/mLDESHUI-JIACHUNRONGYE。
YISHANGLIANGZHONGPEIZHIFANGFA,QIANYIZHONGYINGXIANGYINSUJIAOXIAO,ZHIYUTIANPINGHETIJIDIDINGFASHUIFENCEDINGYIDEWUCHAYOUGUAN,HEJINYANGQI、RONGLIANGPINGWUGUAN,BUQUEDINGDUJIAOXIAO,ZHEIYESHIWOMENYINGYONGBIJIAOHAODEFANGFA。QUEDIANSHIPEIZHILIANGJIAOSHAO,SHOUKONGQIZHONGSHUIFENDEYINGXIANGJIAODA,ZUIHAOZAITIANQIGANZAOSHIPEIZHI。PEIZHICHENGZHILIANGBI,TIJIJINYANGSHIBIXUCHENGYI0.792MIDUXISHU, DANGRANYEKEYIYONG0.792MIDUXISHUHUANSUANPEIZHICHENG10mg/mLDESHUI-JIACHUNRONGYE,ZHEIZAITIJIJINYANGSHIJIAOWEIFANGBIAN。ZAIPEIZHIGUOCHENGZHONG,XUANZETIJIDIDINGFASHUIFENCEDINGYIDEYUANYINSHIYINWEICEDINGJIACHUNDEBENDIHANSHUILIANGSHI,BIXUJIADAJINYANGLIANG(YOUSHIXUJINmLJIDEJIACHUN)CAINENGZHUNQUECECHUBENDISHUIHANLIANG,ERKULUNFASHUIFENYIZAIDAJILIANGJIARUJIACHUNSHI,DIANJIEYEPEIBIFASHENGJIAODAGAIBIAN,RONGYIZAOCHENGCEDINGKAISHISHIDELINGDIANHECEDINGHOUDELINGDIANBUTONG,WUCHAYUECEYUEDA。ERTIJIDIDINGFASHUIFENCEDINGYIKAISHIDIDINGSHIYONGDEJIUSHICHUNJIACHUN,JIADAJINYANGLIANGYEBUHUICHUXIANCELIANGWUCHAZENGDADEQINGKUANG。YONGSHANGSHUFANGFACEDINGJIACHUNBENDISHUIFENSHI,DANGWENDINGCEDEYIGEZHISHI,YINGDANGZAIJIADAJINYANGLIANGCELIANG,YIYANZHENGBENDISHUIFENDECELIANGSHIFOUZHUNQUE;DANGJINGJISUANTIANJIASHUIFENHOUZAIJINXINGFANCE,TONGYANGKEYIYANZHENGYIQIDESHIZHIWUCHA,ZHEIZAIYIHOUDEBUQUEDINGDUJISUANZHONGYONGDAO。JINGDUIBUQUEDINGDUDEJISUAN,JIEGUOMANZUGUICHENG(U=1.4,k=2)DEYAOQIU。
ZUOZHEDANWEI【SHANDONGSHENGJILIANGKEXUEYANJIUYUAN】