金属螺钉六价铬处理的定量测定

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本申请说明描述了使用显色反应和紫外可见光谱法从两个螺钉样品的处理中提取和定量残留铬。 关键词:V-630,UV-可见/NIR,材料,IEC-62321,29CFR第1910部分,29CFR第1915部分

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通过水热萃取法从两个钢螺钉中提取铬。将螺钉置于25mL纯化水中,并在80摄氏度下加热30分钟。这些条件可能会根据样品类型和法规遵从性而发生变化。Application Note Quantitative Measurement of HexahydricChromium Treated to Screws2/3 UV-0015 Quantitative Measurement of Hexavalent Chromium Treatment to Metal Screw s In t ro d uc t ion Hexavelent chromium (Cr(VI)) is a sign i ficantly hazardous material regu l ated by OSHA wi t h r efe r ence to 29CFR p arts 1910 a nd 1915, by RoHS direct i ve, and by I EC -62321wh i c h st r ictly con t rols and reg u lates the use of specif i c h azardous materials in a wide range o f industr i al processes as well as electr i cal and electronic products. This application n ote descr i bes the extraction and q u anti f ication of residual chromium from the treatment o f two samples of screws us i ng a chromogenic reaction and UV-Visible spectroscopy. V-630 UV-Visible Spectrophotomete r The chromium f r om two steel screws (F i gure 1) was extrac t ed via Hydrot h ermal Extract i on. T h e screws were p laced in 25 mL of pu rif ied wate r and heated at 80 degrees Cels i us f or 30 minutes. These cond iti ons are sub j ect to cha n ge dependi n g on t h e samp l e type a n d regulatory compliance Keywords V-630,U V -V i si bl e/NIR , M a t e ri a l s, IE C-62321, 29C F R p ar t 1910, 29C F R p a r t 1915 Exper i mental T h e chrom iu m f r om t wo steel sc r e ws (Fig u re 1) was e xtra c t ed via Hydrot h ermal Ext r ac ti on. The screws were placed i n 25 mL of puri f ied water and heated at 80 degrees Celsius for 30 minu t es. These co n ditions are subject to change depe n ding on the chromium coati n gs for a par t icular sc r ew. Appl i c a t i on Note Figure 1. Sam p l e s cr ew s. Afte r hydrot h ermal extra c t i on, the screws were removed f rom the extract i o n liq u id which was cooled to room temperatu r e. The chromogen i c r eagent (Kyoritsu Chem i cal -C h eck Lab) was added to the ext r action liquid, st i rred for 1 minute, and the l eft to stand for 5 mi n utes. Turbidity was observed after 5 m i nutes. Fig u re 2 shows t h e sample pre-and post-filtration. Measurements were obtained on both samples for compar i son using the f ollowing measurements parameters. Measurement Conditions Bandwidth 1.5nm Data Interval 0.2nm Scan Speed 400 nm/min Response Medium Figure 2. Sc rew samp le s af ter t h e chro m og eni c ag en t w as a dde d t o t he e xtr a ction solution s and p r e- (le ft ) f ilt ra ti on an d post (r igh t) filt r atio n o f t he sol u t ions . 28600 Mary's Cour t , E a s to n , M D 21601US A UASGO A ppli c a tio n Lib r ary: htt p://www.jas co in c .c o m/a pp l icatio n s Res ul ts The spec t ra of t he samples before a n d after f iltrat i o n are i l lustra t ed in F i gure 3. T he s p ec t r u m of t h e sample before filtra t ion shows a highe r b asel in e, which i s due to the dispe r sion o f interferin g substa n ces in t h e solu t ion. A t h ree wavelength quant i tative analysis was performed to conf i rm the effects of the interfe r i ng substa n ces. Table 1 shows t he results of the peak height calcu l at i ons. Rega r dless of the pretreatment, almost identical results we r e obtained. Figure 3. A b s or pt ion spect ra of s a m pl es A a nd B bef or e (p ur p l e) a n d a f ter (b lue) f i l t ra tio n . Table 1. P e ak h eight calc ul at i o n r e s ul ts of scr e w s am pl e s A and B . Sample A Sample B Before After Before After 1 Wavelength Abs at 542 nm 0.10393 0.09288 0.06365 0.04482 3 Wavelength Peak height: 542 nmBase: 402, 635nm 0.08782 0.08765 0.03932 0.03915 Three wave l e n gth qua n titative a n alysis was examined on the p eak h eight calc u lated with p e a k wave l ength at 402nm and a base wavelength at 635 a nd 542 nm. The calibration c u rve obtained by the diphenylcarbazide method i n Application Note UV-0004 was appl i ed to t h is quan ti tative analysis. Table 2 shows the concentration of Cr (VI) for samples A and B using a two-sided 95% confidence interval and both samples A and B fall wi th in ±0.005 mg/L of the conf i dence i nte r val . Table 2. Qu an tit a t i v e r e s ults o f C r (Vl ) i n s c r e w sa m p l e s. Sample A Sample B Before After Before After 0.135±0.006 mg/L 0.135±0.006 mg/L 0.059±0.005 mg/L 0.059±0.005 mg/L JASCO INC. 28600 Mary's Cour t , E a s to n , M D 21601US A

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