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Ê×ÏȽ«²»Í¬Ìå»ýµÄÑùÆ·ÈÜÒº¼ÓÈëµÎ¶¨±ÖУ¬²¢ÓÃÈ¥Àë×ÓË®¶¨ÈÝÖÁ40ml¡£¼ÓÒºÍê³ÉºóÓñ궨ºóµÄNaOHÈÜÒºµÎ¶¨£¬µÃµ½µÎ¶¨ÖÕµãºóÁ¢¼´Í£Ö¹¡£´ËʱµÎ¶¨ÖÕµãָʾµÄNaOHÈÜÒºÏûºÄÁ¿ÓÃÓÚ¼ÆËãÈÜÒºÖеÄH+¡£Ëæºó£¬ÔÚͬһµÎ¶¨±ÖмÓÈë10mlÀë×Ó»º³åÒº£¬½Á°è¾ùÓ룬Óñ궨ºóµÄNaFÈÜÒºµÎ¶¨£¬µÃµ½µÎ¶¨ÖÕµãºóÍ£Ö¹¡£´ËʱµÎ¶¨ÖÕµãָʾµÄNaFÈÜÒºÏûºÄÁ¿ÓÃÓÚ¼ÆËãÈÜÒºÖеÄAl3+¡£
±¾ÎÄÉæ¼°µÄ¸öÑùÆ·ÖУ¬SH-1ºÍSH-2ºÅÑùÆ·Ö»Ðè×ö*²½£¬SAl-1ºÅÑùÖ»Ðè×öµÚ¶þ²½£¬SM -1¡¢SM-2ºÅ¼°Êµ¼ÊÑùÆ·ÔòÐèÏÈ×ö*²½ÔÙ×öµÚ¶þ²½¡£
1.5 ¹«Ê½
µÎ¶¨¶È¼ÆË㹫ʽ
×ÜËá¶È£ºC=(VNaOH-blank)*CNaOH/Vsample
Al3+Ũ¶È£ºC=(VNaF-blank)*CNaF/Vsample
ÆäÖУ¬VNaOHºÍVNaF·Ö±ðÖ¸µ½´ïµÎ¶¨ÖÕµãʱÏûºÄµÎ¶¨¼ÁµÄÌå»ý£»blankÖ¸²»Í¬·½·¨¶ÔÓ¦µÄ¿Õ°×Öµ£»CNaOHºÍCNaF·Ö±ðÖ¸±ê¶¨ºóµÎ¶¨¼ÁµÄŨ¶È£»Vsample´ú±í½øÑùÁ¿¡£
2 ½á¹ûÓëÌÖÂÛ
ζȵζ¨Èí¼þ²ÉÓù¦ÄÜÇ¿¡¢ÒÔ¹ýÂËϵÊýΪ±äÁ¿µÄÊý×ÖÆ½»¬Ëã·¨º¯Êý£¬¿ÉʹµÈµ±µãÆ¯ÒÆzuiС»¯¡£¶ÔÓÚÑϽ÷µÄÓÅ»¯£¬Ó¦¸Ã¿¼ÂǹýÂËϵÊý¶ÔµÈµ±µãµÄÓ°Ïì[7]¡£Ñ¡ÔñºÏÊʵĹýÂËϵÊýʹµÈµ±µãÌå»ýÎȶ¨¡£²»Í¬µÄ·½·¨¶¼Òª¿¼ÂǹýÂËϵÊýµÄÓ°Ïì¡£
2.1 ¹ýÂËϵÊýµÄÈ·¶¨
¶ÔÓÚNaOH±ê¶¨ÊÔÑ飬ÎÒÃÇ¿¼²éÁ˹ýÂËϵÊýΪ20¡¢30¡¢40¡¢50¡¢60¡¢70¡¢80¡¢90¡¢100ºÍ110ʱÏûºÄµÎ¶¨¼ÁÖÕµãµÄÌå»ý£¬±í2ÏÔʾѡÔñ¹ýÂËϵÊýΪ50zuiÊʺϡ£±ê¶¨NaFÊÔÑé¹ýÂËϵÊýµÄÑ¡ÔñÓëÉÏÊöÏàËÆ£¬zuiºóÑ¡ÔñµÄ¹ýÂËϵÊýÒ²ÊÇ50¡£
±í2 ¹ýÂËϵÊýµÄÓÅ»¯
Table 2 Optimization of filter factor
Filter factor
20
30
40
50
60
70
80
90
VEP(ml)
7.85
7.85
7.85
7.85
8.01
8.29
8.27
8.96
2.2 ¿Õ°×ÖµµÄÈ·¶¨
Ó봫ͳµÎ¶¨²»Í¬£¬Î¶ȵζ¨ËùÐèÒªµÄζÈÐÅÏ¢Æä´«Ëͺʹ¦Àí¶¼´æÔÚÒ»¶¨µÄʱ¼äÑÓ³Ù£¬ÓÉÓڵζ¨¹ý³ÌΪºãËٵζ¨¹ý³Ì£¬Òò´ËÕâÑùµÄʱ¼äÑÓ³Ù£¬¿ÉÒÔ±íʾΪһ¶¨Ìå»ýµÄµÎ¶¨¼Á£¬¼´Î¶ȵζ¨·½·¨µÄ¿Õ°×Öµ¡£·½·¨¿Õ°×µÄ²âÁ¿ÊÇÓò»Í¬Å¨¶ÈµÄ±»²âÎïÔÚÏÈǰÓÅ»¯ºÃµÄÌõ¼þϽøÐе樣¬½«±»²âÎïŨ¶ÈÓëµÎ¶¨¼ÁÏûºÄµÄµÈµ±µã×÷ͼ¡£·½·¨µÄ¿Õ°×Öµ£¬¼´ÎªÓÃËù²âµÄµÎ¶¨Êý¾Ý×÷ÏßÐԻعéµÄyÖá½Ø¾à¡£¸Ä±ä·½·¨µÄ²ÎÊý¾ÍÒªÇóÖØÐÂ×÷·½·¨µÄ¿Õ°×Öµ¡£Òò´Ë±¾ÎÄÖб궨NaOHºÍÓÃNaOHµÎ¶¨×ÜËá¶È¾ùÐè×ö±ê×¼ÇúÏߣ»¶ø±ê¶¨NaFËù×÷µÄ±êÇú¿ÉÒÔÖ±½ÓÓ¦ÓÃÓÚÖ®ºóµÄAl3+²â¶¨¡£
È·¶¨¹ýÂËϵÊýºó£¬°´ÕÕÉÏÊöÊÔÑé·½·¨ÖеIJ½Ö裬¿ÉÒԵõ½NaOH±ê¶¨µÄ±ê×¼ÇúÏߺÍNaFµÎ¶¨Al3+µÄ±ê×¼ÇúÏß¡£
ͼ1 NaOH±ê¶¨±ê×¼ÇúÏß
Fig. 1 Standard curve for NaOH
´Óͼ1ÖпÉÒÔ¼ÆËã³ö£¬CNaOH=1/0.518=1.93mol/L£¬¿Õ°×Öµ¼´yÖá½Ø¾à0.0192ml¡£
ͼ2 NaF±ê¶¨µÄ±ê×¼ÇúÏß
Fig. 2 Standard curve for NaF
ÓÉÓÚ1mol Al3+ºÍ6mol F-·´Ó¦£¬ËùÒÔCNaF=6/5.2094=1.15mol/L£¬¿Õ°×ֵΪyÖá½Ø¾à0.0457ml¡£
2.3 Ä£ÄâÑùÆ·²âÊÔ½á¹û
ʵÑé½á¹û±íÃ÷SH-1£¬SH-2£¬SAl-1ºÅÑùÆ·µÄŨ¶È·Ö±ðΪCSH-1=7.23M£¨RSD=0.35£©£¬CSH-2=5.5M£¨RSD=0.19£©£¬CSAl-1=0.48M(RSD=0.52)£»SM-1ºÍSM-2ºÅ½á¹ûÈç±í3Ëùʾ¡£
±í3 ±êÑùSM-1ºÍSM-2ÑùÆ·ÖÐ×ÜËá¶ÈºÍAl3+Ũ¶ÈµÄƽ¾ùÖµºÍÏà¶Ô±ê׼ƫ²î
Table 3 Measurement results of different samples
ÀíÂÛÖµ
Certified
񅧏
No.
C(mol/L)
Mean (mol/L)
RSD£¨%£©
Sample SM-1
(C(H+)=7.23
mol/L)
1
7.31
7.26
0.39
2
7.24
3
7.24
4
7.27
5
7.27
Sample SM-1
(C( Al3+)=0.48
mol/L)
1
0.49
0.49
0.63
2
0.50
3
0.49
Sample SM-2
(C(H+)=5.5
mol/L)
1
5.40
5.43
0.50
2
5.42
3
5.43
4
5.47
5
5.44
Sample SM-2
(C(Al3+)=0.48
mol/L)
1
0.47
0.47
0.19
2
0.47
3
0.47
´Ó½á¹û¿ÉÒÔ¿´³ö£¬¶ÔÓÚÁ½¸ö×ÔÅäµÄ±êÑùSM-1ºÍSM-2£¬×ÜËá¶ÈºÍAl3+Ũ¶È²â¶¨½á¹ûºÍÀíÂÛÖµ·ûºÏ£¬ÁéÃô¶È¸ß£¬ÖØÏÖÐԺã¬RSD¾ùÔÚ1%ÒÔÄÚ¡£
2.3 ¾«ÃܶȲâÊÔ
¶ÔÓÚ±ê×¼ÑùÆ·2£¬²â×ÜËá¶ÈʱÁ¬ÐøµÎ¶¨15´Î£¬ ²âAl3+ʱÁ¬ÐøµÎ¶¨5´Î£¬½á¹ûÈç±í4£¬¸Ã·½·¨¾«ÃܶȺܺã¬RSD¾ùÔÚ1%ÒÔÄÚ¡£
±í4 ¾«ÃܶÈʵÑé
Table 4¡¡Analytical results of sample SM-1
ÀíÂÛÖµ
Certified
񅧏
No.
C(mol/L)
Mean (mol/L)
RSD£¨%£©
Sample SM-1
(C(H+)=7.23
mol/L)
1
7.32
7.26
0.39
2
7.29
3
7.32
4
7.21
5
7.26
6
7.24
7
7.23
8
7.23
9
7.25
10
7.25
11
7.28
12
7.28
13
7.26
14
7.28
15
7.27
Sample SM-1
(C(Al3+)=0.479 mol/L)
1
0.49
0.49
0.88
2
0.50
3
0.49
4
0.50
5
0.49
2.4 ¼Ó±ê»ØÊÕ
¶Ô×ÔÅäµÄ±ê×¼ÑùÆ·2½øÐÐÁË¼Ó±ê»ØÊÕµÄʵÑ飬±í5ÏÔʾ£¬»ØÊÕÂʾùÔÚ95%-105%Ö®¼ä£¬RSD¾ùÔÚ4%ÒÔÄÚ¡£
±í5 ±êÑùSM-1ÖÐH+ºÍAl3+Ìí¼ÓʵÑ黨ÊÕÂʺÍÏà¶Ô±ê׼ƫ²î
Table 5 Recovery test for H+ and Al3+
씀items
񅧏
No.
ÔÑù
(mmol)
Original
ÀíÂÛ¼Ó±êÁ¿
(mmol)
Added
»ØÊÕÁ¿
(mmol)
Recovered
»ØÊÕÂÊ
(%)
Recovery
RSD
(%)
H+
1
5.808
6.312
6.762
3.9
2
7.26
7.89
7.87
3
7.986
8.679
8.664
100.26
4
8.712
9.468
9.448
5
10.89
11.835
11.26
Al3+
1
0.395
0.382
0.416
3.4
2
0.494
0.478
0.498
3
0.543
0.526
0.546
103.74
4
0.593
0.574
0.598
5
0.741
0.717
0.701
2.5 ʵ¼ÊÑùÆ·²âÊÔ½á¹û
zuiºó£¬±¾ÎĽ«¸Ã·½·¨Ó¦Óõ½Õë¶ÔijÂÁ³§µç½â²Û·ÏË®µÄʵ¼Ê¼ì²âµ±ÖС£ÊµÑé½á¹û±íÃ÷£¬¸ÃÑùÆ·µÄH+Ũ¶ÈΪ7.37M£¬RSD=0.67%£»Al3+Ũ¶ÈΪ0.512M£¬RSD=0.46%¡£¸Ã½á¹ûÓëÑùÆ·Ìṩµ¥Î»µÄ²â¶¨½á¹û·ûºÏ¡£ÕâÑùµÄ½á¹û½øÒ»²½Ö¤Ã÷ÁË£¬»ùÓÚζȵ樵Äз½·¨¿ÉÒÔÔÚʵ¼ÊÑùÆ·²â¶¨ÖÐÆðµ½½ÏºÃµÄЧ¹û¡£
3 ½áÂÛ
±¾ÊµÑé²ÉÓÃζȵζ¨µÄ·½·¨£¬¶ÔÂÁ²Ä±íÃæ´¦Àí·ÏË®ÖеÄ×ÜËá¶ÈºÍAl3+Ũ¶È½øÐÐÁ˶¨Á¿·ÖÎö¡£½á¹û±íÃ÷£¬´Ë·½·¨ÓнϸߵÄ׼ȷ¶ÈºÍÁéÃô¶È£¬ÇÒÆ½ÐÐÐԺá£ÔÚÕû¸ö²âÁ¿ÖУ¬Á½¸öµÎ¶¨ÏîÄ¿¿ÉÔÚͬһµÎ¶¨±ÖÐÍê³É¡£ÓëÒÔÍù·½·¨Ïà±È£¬¸Ã·½·¨Ïû³ýÁËÈ¡Ñù¹ý³ÌºÍµÎ¶¨¹ý³ÌÖÐËù²úÉúµÄÎó²î£»Í¬Ê±ÔÚÓ빫˾Éú²úµÄ815×Ô¶¯½øÑùÁªºÏʹÓú󣬿ɴó´óÌá¸ß¹¤×÷ЧÂÊ£¬ÌرðÊʺÏÑùÆ·Á¿½Ï´óµÄÓû§¡£
²Î¿¼ÎÄÏ×
[1] Îâ¡¡Ãô, Ëï¡¡ÓÂ. ÂÁ¼°ÆäºÏ½ð±íÃæ´¦ÀíµÄÑо¿ÏÖ×´[J]. ±íÃæ¼¼Êõ(Surface Technology), 2003, 32 (3): 13-15.
[2]Zhou W Q, Shan D, Han E H, et al. Structure and formation mechanism of phosphate conversion coating on diecast AZ91D magnesium alloy [J]. Corrosion Science, 2008, 50 (2): 329-337.
[3] Watkims K G, Liu Z , Memahon M , et al . Influence of the over lapped area on t he corrosion behaviour of laser treated aluminum alloy[J] . Materials Science and Engineering, 1998, A252 : 292-300.
[4]ÕŸ߻á, »Æ¹úÇà, ÐìÅô, µÈ. ÂÁ¼°ÂÁºÏ½ð±íÃæ´¦ÀíÑо¿½øÕ¹[J]. Öйú¼ÆÁ¿Ñ§ÔºÑ§±¨(Journal of China Jiliang University), 2010, 21(2): 174-178.
[5] »ÆÄÈɯ, ÄßÒæ»ª, ÑÐÂ, µÈ. ÂÁºÏ½ð±íÃæ¸ÄÐÔ¼¼ÊõµÄÑо¿Óë½øÕ¹[J]. ÇṤ»úе(Light Industry Machinery), 2010, 28(4): 4-11.
[6]Áõºê, ÏòÔ¢»ª, Áõ±ÌÐÛ. ÂÁÐͲıíÃæ´¦Àí·ÏË®ÖÎÀíµÄ¹¤ÒÕÌõ¼þ̽Ë÷[J]. µç¶ÆÓëÍ¿ÊÎ(Electroplating and Finishing), 2008, 27(9): 34-36.
[7]ÌÆº£·å, ÌÆ»ù», ÀîѸ. ÂÁºÏ½ð±íÃæ´¦ÀíµÄ·ÏË®ÖÎÀí[J]. µç¶ÆÓ뾫ÊÎ(Plating & Finishing), 2005, 27(2): 46-48.
[8] Öì׿·¼. ½¨ÖþÂÁÐͲĵıíÃæ´¦Àí¼¼ÊõÏÖ×´¼°·¢Õ¹Ç÷ÊÆ[J]. µç¶ÆÓëÍ¿ÊÎ(Electroplating and Finishing), 2005, 24 (4): 14-17.
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Determination of TAN and Aluminium in waste water of Surface treatment by Thermometric Titration
Abstract: In this paper, a new method based on thermometric titration was developed for H+ and Al3+determination. Under the new method, the concentration of H+ and Al3+ could be determined in same vessel after one sampling. The recovery and relative standard deviation (RSD) were 99.79% to 104.06% and 0.39% to 0.88% respectively. The new method was accurate, reproducible and simple. Our result also proved that this method could be used in the determination of H+ and Al3+ in waste water come form aluminum industry
Key words: Thermometric titration; Aluminum; Acid treatment; Enthalpy
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HI96701
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HI93707
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HI96715
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HI96717
HI93717
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HI96721
HI93721
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