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±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

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2.1 ¹ýÂËϵÊýµÄÈ·¶¨

¶ÔÓÚNaOH±ê¶¨ÊÔÑ飬ÎÒÃÇ¿¼²éÁ˹ýÂËϵÊýΪ20¡¢30¡¢40¡¢50¡¢60¡¢70¡¢80¡¢90¡¢100ºÍ110ʱÏûºÄµÎ¶¨¼ÁÖÕµãµÄÌå»ý£¬±í2ÏÔʾѡÔñ¹ýÂËϵÊýΪ50zuiÊʺÏ¡£±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+

씀
items

񅧏

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.

[9] ÈðÊ¿Íòͨ. ²úÆ·Ñù±¾—859ζȵζ¨ÒÇ[J]. ÈðÊ¿ÍòͨÄÚ²¿ÎÄÏ×.

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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HI96716

HI93716

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HI96701

HI93701

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HI96706

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HI96707

HI93707

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