DOCSLIB.ORG

Alcohols Combined 1405

Total Page：16

File Type：pdf, Size：1020Kb

Download full-text PDF Read full-text

Load more

  • ALCOHOLS COMBINED
  • 1405

  • Formulas: Table 1
  • MW: Table 1
  • CAS: Table 2
  • RTECS: Table 2

  • METHOD: 1405, Issue 1
  • EVALUATION: PARTIAL
  • Issue 1: 15 March 2003

OSHA : Table 2 NIOSH: Table 2 ACGIH: Table 2
PROPERTIES:

Table 1

COMPOUNDS:

(1) n-butyl alcohol (2) sec-butyl alcohol (3) isobutyl alcohol
(4) n-propyl alcohol (5) allyl alcohol (6) diacetone alcohol
(7) cyclohexanol (8) isoamyl alcohol (9) methyl isobutyl carbinol

SYNONYMS: See Table 3.

  • SAMPLING
  • MEASUREMENT

SAMPLER:

SOLID SORBENT TUBE (Coconut shell charcoal, 100 mg/50 mg)

TECHNIQUE: ANALYTE:

GAS CHROMATOGRAPHY, FID Compounds above

FLOW RATE: 0.01 to 0.2 L/min
DESORPTION:

1 mL 5% 2-propanol in CS2
Compounds: (1-3 )

(4-9)

1 L

INJECTION VOLUME:
VOL-MIN:
-MAX:

2 L

  • 1 µL
  • 10 L
  • 10 L

SHIPMENT: Routine
TEMPERATURE
-INJECTION: 220 °C

-DETECTOR: 250 - 300 °C
SAMPLE STABILITY: See Evaluation of Method.

-COLUMN:

35 °C (7 minutes), to 60 °C at 5 °C/minute, hold 5 minutes, up to 120 °C at 10 °C /minute, hold 3 minutes.

BLANKS:

2 to 10 field blanks per set

CARRIER GAS: COLUMN:

He, 4 mL/min

ACCURACY

Capillary, fused silica, 30 m x 0.32-mm ID; 0.5 µm film polyethylene glycol, DB- wax or equivalent

RANGE STUDIED: Not studied [1, 2]. BIAS:

Not determined

CALIBRATION: RANGE:

Solutions of analyte in eluent (internal standard optional)

OVERALL PRECISION (ÖrT): Not determined

See EVALUATION OF METHOD.

ACCURACY: Not determined
ESTIMATED LOD: 1 µg each analyte per sample

PRECISION: See EVALUATION OF METHOD.

APPLICABILITY: This method may be used to determine two or more of the specified analytes simultaneously. INTERFERENCES: High humidity reduces sampling capacity. Less volatile compounds may displace more volatile compounds on the charcoal.

OTHER METHODS: This method combines and updates Methods 1401 and 1402, NMAM, Fourth Edition, Issue 2. Estimated LOD for each analyte is approximately ten times lower than that of the old methods.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 2 o f 6

  • EQUIPMENT:
  • REAGENTS:

1. S a m ple r: Gla s s tube , 7-cm long, 6-mm OD, 4- mm ID, fla me -s e a le d e nds, containing two se ctio ns of a ctivate d (6 00 °C) coc on ut s he ll cha rcoa l (front - 100 mg; ba ck - 50 mg) s e pa ra te d by a 2-mm ure tha ne foa m plug follows the ba ck s e ction. P re s s ure drop a cros s the tube at 1 L/min a irflow mus t be le s s tha n 3.4 kPa . Tub es are com m ercia lly a va ila ble .
2. P e rs ona l s a mpling pump, 0.01 to 0.2 L/min, with fle xible conne cting tubing.
3. Ga s chroma togra ph, FID, inte gra tor a nd colum n (pa ge 14 05-1).
1. Ca rbon disulfide, ch rom atog raph ic gra de.* 2. 2-P ropa nol, ch rom atog raph ic gra de.* 3. He xan e, ch rom atog raph ic gra de.* 4. He ptan e, ch rom atog raph ic gra de.* 5. De s orbing s olution: Ca rbon dis ulfide with 5%
(v/v) 2-propa nol a nd 0.05% (v/v) he xa ne a s a n inte rna l s ta nda rd. NOTE: n-Unde ca ne , 0.1 (v/v) or othe r s uita ble s ta nda rd ca n be us e d.
6. Ana lyte (s ). 7. S tock s olution, 100 mg/mL. P re pa re s olutions of e a ch a na lyte in he pta ne .
8. Nitroge n, purifie d.
4. Via ls , gla s s , 2-mL, P TFE -line d crimp ca ps . 5. S yringe , 10-µL, rea da ble to 0.1 µL. 6. Volume tric fla s ks , 2 mL.
9. Hydroge n, pre purifie d.
10. Air, compre s s e d, filte re d.

* Se e SP ECIAL P RECAUTIONS

SPECIAL PRECAUTIONS: Ca rbon dis ulfide is toxic a nd a n a cute fire a nd e xplos ion ha za rd (fla s h point = -30 °C); a ll work with it mus t be done in a hood. P ropa nol, he xa ne , a nd he pta ne a re fla mm a ble . Ana lyte s s hould be ha n dle d in a fume hood. W e a r glove s , s a fe ty gla s s e s , a nd a pp ropria te prote ctive clothing.

SAMPLING:

1. Ca libra te e a ch pe rs ona l s a mpling pump with a re pre s e nta tive s a mple r in line . 2. Bre a k the e nds of the s a mple r imm e dia te ly be fore s a mpling. Atta ch s a mple r to pe rs ona l s a mpling pump with fle xible tubing.
3. Sa m ple at a n ac curately kn own flow ra te be twee n 0.0 1 an d 0.2 L/m in for a total sa m ple size of 1 to
10 L (2 to 10 L for n-buta n ol, s e c-buta nol, a nd is obutyl a lcohol).
4. Ca p the sam plers with pla stic (not rub ber) cap s an d pa ck sec urely for shipm ent.

SAMPLE PREPARATION:

5. P la ce the front a nd ba ck s orbe nt s e ctions of the s a mple r tube in s e pa ra te via ls . Dis ca rd the gla s s wool a nd foa m plugs .
6. Ad d 1.0 m L des orbing s olution (DS) to e ac h vial. Attac h crim p cap to e ac h vial. 7. Allow to s ta nd 30 min with occa s iona l agita tion.

CALIBRATION AND QUALITY CONTROL:

8. Ca libra te da ily with a t le a s t s ix working s ta nda rds covering the ra nge of s a mple s . a . Add known am oun ts of a nalyte to DS in 2-m L volum etric flas ks and dilute to th e m ark. b. Ana lyze toge the r with s a mp le s a nd bla nks (s te ps 11 a nd 12). c. P re pa re ca libra tion graph (ra tio of pe a k a rea of ana lyte to pe a k a re a of inte rna l s tanda rd vs . µg a na lyte .
9. Dete rm ine de so rption efficie nc y (DE) at le as t on ce for ea ch ba tch of c ha rcoa l us ed for sa m pling in the ca libra tion ra nge (s te p 8). P repa re thre e tube s a t e ach of five le ve ls plus tre e me dia bla nks . a . Re m ove a nd dis ca rd ba ck s orbe nt s e c tion of a me d ia bla nk s a m ple r. b. Inje ct a known a mount of s tock s olution dire ctly onto front s orbe nt s e ction with a microlite r s yringe .

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 3 o f 6 c. Ca p the tube . Allow to stan d overnig ht. d. De s o rb (s te ps 5 through 7 ) a nd a na lyze toge the r with working s ta nda rds (s te ps 11 a nd 12). e . P re pa re a gra ph of DE vs . µg a na lyte re cove re d.
10. Ana lyze thre e qua lity control bind s pike s a nd thre e a na lys t s pike s to ins ure tha t the ca libra tion gra ph an d DE g ra ph are in con trol.

MEASUREMENT:

11. S e t ga s chroma togra ph a ccording to ma nufa cture r’s re comm e nda tions a nd to conditions give n on pag e 14 05-1 . Inject s am ple aliqu ot m anu ally using solve nt flus h tec hnique o r with a utos am pler. NOTE: If pea k a rea is abo ve the linear ra nge of the working stan dard s, dilute with elue nt, re a na lyze , a nd a pply the a ppropria te dilution fa ctor in calcula tions .
12. Me a s ure pe a k a re a . Divide the pea k a re a of a na lyte by the pe a k a re a of inte rna l s ta nda rd on the s a me chrom a togra m.

CALCULATIONS:

13. De te rm ine the ma s s , µg (corre c te d for DE) of a n a lyte found in the s a m ple front (Wf) a nd ba ck (W b) s orbe nt s e c tions a nd in the a ve ra ge m e dia bla nk front (Bf) a nd (Bb) sorben t sec tions. NO TE: If W b > Wf/10, re port bre a kthrough a nd pos s ible s a mple los s .
14. Ca lcula te conce ntra tion, C, of a na lyte in the a ir volume s a m ple d, V (L):

NO TE : :g/L = m g/m 3

EVALUATION OF METHOD:

P re vious Eva lua tions [2] This me thod, NIOS H 1405, combine s a nd upda te s NIOS H Me thods 1401 a nd 1402. Me thods 1401 a n 1402 we re ba s e d on the 2nd e dition NMAM Me thods S 66 (n-butyl a lcohol), S 53 (s e c-butyl a lcohol), S 64 (is obutyl a lcohol), S 62 (n-propyl a lcohol), S 52 (a llyl a lcohol), S 55 (dia ce tone a lcohol), S 54 (cyclohe xa n ol), S 58 (is oa myl a ocohol), a nd S 60 (me thyl is obutyl ca rbinol) which we re is s ue d on J a nua ry 17, 1975 [3] a nd va lida ted us ing 10-L air s am ple s of atm os ph eres ge ne ra ted by injec tion of the pure alcoh ol into d ry air us ing a ca libra te d s yringe drive [1]. No s tora ge s ta bility s tudie s we re pe rforme d. Ove ra ll pre cis ion a nd re cove rie s a re s hown Ta ble 4, re pre s e nting non-s ignifica nt bia s in e a ch me thod.

  • Curre nt Eva lua tion
  • [4]

Meth od s for alcoh ols (n-bu tyl alc oh ol, s ec -butyl a lco ho l, iso bu tyl alc oh ol, n -propyl a lco ho l, allyl a lco ho l, dia ce tone a lcohol, cyclohe xa nol, is oa myl a lcohol) we re e va lua te d us ing a na lyte s fortifie d on Ana s orb CS C s orbe nt tube s (Lot #2000). Ta ble 5 lis ts the de s orption e fficie ncy (DE) a nd pre cis ion for the compounds te s te d in the e va lua tion.

S tora ge s ta bility s tudie s we re pe rforme d a t two differe nt conce ntra tion le ve ls : one a t a pproxima te ly 10 µg e a ch a na lyte /s a mple for the low le ve l, a nd the othe r a t a pproxima te ly 150 µg e a ch a na lyte /s a mple for the high le ve l. The sa m ple s were s tored for 7, 1 4, 2 1, a nd 30 da ys a t 5 °C. The res ults are sum m arized in Ta ble 5.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 4 o f 6

REFERENCES:

[1] NIOS H [1977]. Docum e nta tion of the NIOS H Va lida tion Te s ts . Cincinna ti, OH: U.S . De pa rtme nt of
He a lth, Educa tion, a nd We lfa re , P ubl. (NIOS H) 77-185.
[2] NIOS H [1994]. Me thods 1401 a nd 1402. In: Elle r P M, Ca s s ine lli ME, e ds . NIOS H Ma nua l of
Analytical Metho ds, 4 th e d. Cincinna ti, OH: Na tiona l Ins titute for Occupa tiona l S a fe ty a nd He a lth, DHHS (NIOS H) P ublica tion No. 94-113.
[3] Ta ylor DG , eds [197 7]. NIO SH Ma nua l of An alytical Metho ds, 2 nd e d., V.2., Cincinna ti, OH: U.S .
De pa rtme nt of He alth, Educa tion, and We lfa re . DHHS (NIOS H) P ublication No. 77-157-B.
[4] Yoon YH, P e rkins J B, Re ynolds J M [2002]. Ba ck-up Da ta Re port for Alcohols Combine d. Da ta Che m
La bora torie s , Inc. unde r NIO S H c ontra cts CDC-200 -95-2955 a nd CDC 200 -2001-080 00 (Augu s t).

METHOD WRITTEN BY:

Yound He e Yoon, P h.D. a nd J a me s B. P e rkins , Da ta Che m La bora torie s , Inc., S a lt La ke City, Uta h.

TABLE 1. PROPERTIES

VP @ 20°C, kPa mg/m3
= 1 ppm @ NTP
Density (g/mL)
BP

  • (°C)
  • (mm Hg)

Compound

n-Butyl alcohol

  • Formula
  • M.W.

CH3 CH2 CH2 CH2 OH;

C4 H1 0 O

3.03 3.03 3.03 2.46 2.37 4.75 4.09 3.60 4.18

  • 74.12
  • 0.810

@ 20 °C
117 99.5 108
0.56 (4.2)
1.7 (13)
1.2 (9) sec-Butyl alcohol Isobutyl alcohol n-Propyl alcohol Allyl alcohol
CH3 CH(OH)CH2 CH3 ;

C4 H1 0 O

74.12 74.12 60.09 58.08 116.16 100.16 88.15 102.18
0.808
@ 20 °C

(CH3 )2 CHCH2 OH;

C4 H1 0 O

0.806
@ 15 °C

CH3 CH2 CH2 OH; C3 H8 O
0.805
@ 20 °C

  • 97
  • 2.0 (15)

2.3 (17) 0.1 (0.8) 0.13 (1.0)
3.7 (28) 0.4 (3)
CH2 =CHCH2 OH;

C3 H6 O2

  • 0.854
  • 96-97

  • 167.9
  • 0.931

@ 25 °C
Diacetone alcohol Cyclohexanol
(CH3 )2 C(OH)CH2 COCH3 ;

C6 H1 2 O2 C6 H1 2 O

  • 0.962
  • 161:

MP=24

Isoamyl alcohol

Methyl isobutyl carbinol
(CH3 )2 CHCH2 CH2 OH;

C5 H1 2 O

0.813
@ 15 °C
132

  • 132
  • (CH3 )2 CHCH2 CH(OH)CH3 ;

C6 H1 4 O

0.802
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

ALC OHOLS CO MBINED: METHO D 140 5, Is s ue 1, da te d 15 Ma rch 200 3 - P a ge 5 o f 6

TABLE 2. GENERAL INFORMATION
Exposure Limits

  • Compound
  • CAS #
  • RETECS #
  • OSHA

(ppm)
NIOSH
(ppm)
ACGIH (ppm)

  • n-Butyl alcohol
  • 71-36-3

78-92-2
EO1400000 EO1750000
100 TWA 150 TWA

  • C 50 (skin)
  • C 50 (skin)

  • 100 TWA
  • sec-Butyl alcohol
  • 100 TWA;

150 STEL

Isobutyl alcohol n-Propyl alcohol
78-83-1 71-23-8
NP9625000 UH8225000
100 TWA 200 TWA

  • 50 TWA
  • 50 TWA

  • 200 TWA;
  • 200 TWA;

  • 250 STEL(skin)
  • 250 STEL (skin)

  • Allyl alcohol
  • 107-18-6
  • BA5075000
  • 2 TWA; (skin)
  • 2 TWA;
  • 2 TWA;

  • 4 STEL (skin)
  • 4 STEL (skin)

(Group 1 Pesticide)

Diacetone alcohol Cyclohexanol
123-42-2 108-93-0 123-51-3
SA9100000 GV7875000 EL5425000
50 TWA 50 TWA 100 TWA

  • 50 TWA
  • 50 TWA

  • 50 TWA (skin)
  • 50 TWA (skin)

  • Isoamyl alcohol
  • 100 TWA;

125 STEL(skin)
100 TWA; 125 STEL

  • Methyl isobutyl carbinol
  • 108-11-2
  • SA7350000
  • 25 TWA; (skin)
  • 25 TWA;
  • 25 TWA;

  • 40 STEL (skin)
  • 40 STEL (skin)

TABLE 3. SYNONYMS
Compound

(1) n-butyl a lcohol (2) s e c-Butyl a lcohol (3) is obutyl a lcohol (4) n-propyl a lcohol (5) a llyl a lcohol

Synonyms

1-bu tan ol; n -buta no l; prop yl ca rbinol. 2-buta nol; me thyl e thyl ca rbinol; 2-hydroxybuta ne . 2-me thyl-1-propa nol; is opropyl ca rbinol; IBA. 1-prop an ol; e thyl c arbinol. 2-prop en -1-ol; 2-prop en ol; vinyl carbinol.
(6) dia ce tone a lcohol (7) cyclohe xa nol
4-hydroxy-4-me thyl-2-pe nta none ; 2-me thyl-2-pe nta nol-4-one . he xa lin; h ydralin; hyd roxyc yclo he na ne ; an ol.

  • (8) is oa myl a lcohol
  • 3-m eth yl-1-buta no l; iso bu tylca rbinol; iso pe ntyl a lco ho l.

  • MIBC ; 4-m eth yl-2-pen tan ol; m eth yl am yl alcoh ol.
  • (9) me thyl is obutyl ca rbinol

Recommended publications
  • Website F Prolonged Or Repeated Exposure Can Cause Drying and ( Or in Your Facility’S RTK Cracking of the Skin

    Website F Prolonged Or Repeated Exposure Can Cause Drying and ( Or in Your Facility’S RTK Cracking of the Skin

    Right to Know Hazardous Substance Fact Sheet Common Name: ISOAMYL ALCOHOL Synonyms: Isopentyl Alcohol; Isobutylcarbinol CAS Number: 123-51-3 Chemical Name: 1-Butanol, 3-Methyl- RTK Substance Number: 1039 Date: April 1999 Revision: March 2008 DOT Number: UN 1105 Description and Use EMERGENCY RESPONDERS >>>> SEE BACK PAGE Isoamyl Alcohol is a colorless liquid with a strong Alcohol-like Hazard Summary odor. It is used in photographic chemicals and pharmaceutical Hazard Rating NJDOH NFPA products, as a solvent, as a flavor in food, and in the HEALTH - 1 manufacture of other chemicals. FLAMMABILITY - 2 REACTIVITY - 0 f ODOR THRESHOLD = 0.042 ppm COMBUSTIBLE f Odor thresholds vary greatly. Do not rely on odor alone to POISONOUS GASES ARE PRODUCED IN FIRE determine potentially hazardous exposures. CONTAINERS MAY EXPLODE IN FIRE Hazard Rating Key: 0=minimal; 1=slight; 2=moderate; 3=serious; Reasons for Citation 4=severe f Isoamyl Alcohol is on the Right to Know Hazardous Substance List because it is cited by OSHA, ACGIH, DOT, f Isoamyl Alcohol can affect you when inhaled and by NIOSH and NFPA. passing through the skin. f Contact can severely irritate and burn the skin and eyes with possible eye damage. f Inhaling Isoamyl Alcohol can irritate the nose, throat and lungs. f Isoamyl Alcohol can cause nausea, vomiting and diarrhea. f Exposure can cause headache, dizziness, lightheadedness, and passing out. f Prolonged or repeated exposure can cause drying and SEE GLOSSARY ON PAGE 5. cracking of the skin. f Isoamyl Alcohol may affect the liver and kidneys. FIRST AID Eye Contact f Immediately flush with large amounts of water for at least 15 Workplace Exposure Limits minutes, lifting upper and lower lids.
  • Chapter 13.Pptx

    Chapter 13.Pptx

    Chapter 13: Alcohols and Phenols 13.1 Structure and Properties of Alcohols C C Alkanes Carbon - Carbon Multiple Bonds Carbon-heteroatom single bonds basic O C C C N C N C X O nitro alkane X= F, Cl, Br, I amines Alkenes Alkyl Halide Chapter 23 OH C C H O C O C C O C C Alkynes phenol alcohols ethers epoxide acidic Chapter 14 H H H C S C C C C S S C C S C C H C C sulfides thiols disulfide H H (thioethers) Arenes 253 Nomenclature of alcohols 1. In general, alcohols are named in the same manner as alkanes; replace the -ane suffix for alkanes with an -ol for alcohols CH3CH2CH2CH3 CH3CH2CH2CH2OH OH butane 1-butanol 2-butanol butan-1-ol butan-2-ol 2. Number the carbon chain so that the hydroxyl group gets the lowest number 3. Number the substituents and write the name listing the substituents in alphabetical order. Many alcohols are named using non-systematic nomenclature H C OH 3 OH OH C OH OH HO OH H3C HO H3C benzyl alcohol allyl alcohol tert-butyl alcohol ethylene glycol glycerol (phenylmethanol) (2-propen-1-ol) (2-methyl-2-propanol) (1,2-ethanediol) (1,2,3-propanetriol) 254 127 Alcohols are classified according to the H R C OH C OH H H degree of substitution of the carbon bearing H H 1° carbon the -OH group methanol primary alcohol primary (1°) : one alkyl substituent R R C OH C OH R R secondary (2°) : two alkyl substituents H R 2° carbon 3° carbon tertiary (3°) : three alkyl substituents secondary alcohol tertiary alcohol Physical properties of alcohols – the C-OH bond of alcohols has a significant dipole moment.
  • A New Approach to Prepare Polyethylene Glycol Allyl Glycidyl Ether

    A New Approach to Prepare Polyethylene Glycol Allyl Glycidyl Ether

    E3S Web of Conferences 267, 02004 (2021) https://doi.org/10.1051/e3sconf/202126702004 ICESCE 2021 A new approach to prepare Polyethylene Glycol Allyl Glycidyl Ether Huizhen Wang1*, Ruiyang Xie1, Mingjun Chen1*, Weihao Deng1, Kaixin Zhang2, Jiaqin Liu1 1School of Science, Xihua University, Chengdu 610039, China; 2Chengdu Jingyiqiang Environmental Protection Technology Co., Ltd. Abstract. The polyethylene glycol allyl glycidyl ether (PGAGE) is an important intermediate for preparing silicone softener that can be synthesized from allyl alcohol polyoxyethylene ether and epichlorohydrin (ECH). The performance parameters including the concentration of ECH, initial boron trifluoride diethyl etherate (BFEE) as well as CaCl2 quality were investigated respectively. The optimum process parameters which can get high capping and low by-product rate are as follows: the ECH concentration is 2.0 M, the initial BFEE concentration is 1.65mM, and the CaCl2 dosage is 1.65g/L. Under these conditions, the maximal yield can be improved to 91.36%, the percent of capping rate is higher than 98.16%, the residual concentration of F- is only 0.63 mg/L. concentrated basic solution, in which the total yield was between 90%~91% by Matsuoka et al. [10] also use the 1 Introduction two-step reaction to synthesize AGE based on the reaction Polyethylene glycol allyl glycidyl ether (PGAGE) and the of allyl alcohol with ECH using BFEE as the catalyst. allyl polyoxyethylene ether (APEG), tethering with both Their results demonstrated that the yield reaches 82% alkene and epoxy groups, are widely used as fabric under the following condition: n (ECH) : n (allyl alcohol): finishing agent [1-2] , reactive diluent [3] , cross-linking (catalysis) = 1: (1~3) : (0.01~0.002).
  • Supporting Information

    Supporting Information

    Supporting Information Section 1 Components of DCM based coating strippers Table 1. Composition of Klean Strip Premium. CAS # Components Concentration 75-09-2 Dichloromethane 70.0-95.0% 67-56-1 Methanol < 5.0% 127087-87-0 Poly(oxy-1,2-ethandiyl) < 5.0% 124-38-9 Carbon dioxide < 5.0% Table 2. Composition of Klean Strip X. CAS # Components Concentration 75-09-2 Dichloromethane 30.0 – 40.0% 67-56-1 Methanol 15.0 – 26.0% 67-64-1 Acetone < 10.0% 1330-20-7 Xylene < 10.0% 108-88-3 Toluene < 10.0% 100-41-4 Ethylbenzene < 5.0% 64-17-5 Ethyl alcohol < 5.0% 67-63-0 Isopropyl alcohol < 5.0% Section 2 Sample preparation for the dwell time test As Figure S1 shows, a gasket was pasted on the conformal coating surface and a sheet of parafilm attached to the back of the printed circuit board to avoid solvent leakage dur- ing the dwell test. Figure 1. Sample preparation for the dwell time test. Section 3 Thickness measurement of coated PCBs Materials and Equipment Printed circuit boards (PCB), acrylic conformal coating, tape, Dektak stylus profiler (Bruker, Arizona, USA). Methods A piece of tape was attached on a PCB before coating. The coating was applied on the PCB using the same method as dip coating in the dwell time test. The PCB was sta- tioned and dried at room temperature for over 24 hours. The tape was then torn out to create a coating step. The PCB was fixed on the detection table using tapes. The stylus scanned from sub- strate to coated area.
  • Multicatalytic, Asymmetric Michael/Stetter Reaction Of

    Multicatalytic, Asymmetric Michael/Stetter Reaction Of

    Multicatalytic, asymmetric Michael/Stetter reaction SPECIAL FEATURE of salicylaldehydes and activated alkynes Claire M. Filloux, Stephen P. Lathrop, and Tomislav Rovis1 Department of Chemistry, Colorado State University, Fort Collins, CO 80523 Edited by David W. C. MacMillan, Princeton University, Princeton, NJ, and accepted by the Editorial Board May 30, 2010 (received for review March 22, 2010) We report the development of a multicatalytic, one-pot, asymmetric Ar Ar Michael/Stetter reaction between salicylaldehydes and electron- N H deficient alkynes. The cascade proceeds via amine-mediated OO 3 OTMS (20 mol %) Me HO Me Michael addition followed by an N-heterocyclic carbene-promoted Me Me 1 Ar = 3,5-(CF3)2C6H3 O intramolecular Stetter reaction. A variety of salicylaldehydes, dou- + O O BF4 N bly activated alkynes, and terminal, electrophilic allenes participate 2 Me 5 Me in a one-step or two-step protocol to give a variety of benzofura- NNC F 4a 6 5 One-Pot Two - Po t none products in moderate to good yields and good to excellent (10 mol %) 93% yield 46% yield NaOAc (10 mol %) 85:15:<1:<1 dr 5:1 dr enantioselectivities. The origin of enantioselectivity in the reaction 86% ee 58% ee CHCl3, 23 C is also explored; E∕Z geometry of the reaction intermediate as well as the presence of catalytic amounts of catechol additive are O found to influence reaction enantioselectivity. O Me * O Me ∣ ∣ catalysis organic synthesis tandem catalysis Me 6 ascade catalysis has garnered significant recent attention Scheme 1. Multicatalytic Michael/Benzoin cascade. Cfrom the synthetic community as a means to swiftly assemble CHEMISTRY complex molecules from simple starting materials with minimal benzofuranones.
  • Title Selective Reduction of Acrolein to Allyl Alcohol by a Vapor Phase

    Title Selective Reduction of Acrolein to Allyl Alcohol by a Vapor Phase

    Selective Reduction of Acrolein to Allyl Alcohol by a Vapor Title Phase Hydrogen Transfer Reaction Author(s) Kunichika, Sango; Oka, Shinzaburo; Sakai, Mutsuji Bulletin of the Institute for Chemical Research, Kyoto Citation University (1966), 44(3): 215-220 Issue Date 1966-10-31 URL http://hdl.handle.net/2433/76125 Right Type Departmental Bulletin Paper Textversion publisher Kyoto University Selective Reduction of Acrolein to Allyl Alcohol by a Vapor Phase Hydrogen Transfer Reaction Sango KUNICHIKA,Shinzaburo OKA and Mutsuji SAKAI* (KunichikaLaboratory) (ReceivedJune 15, 1966) Selectivereduction of acroleinto ally! alcoholhas been achievedby a vapor phase hydrogen transferreaction using isopropyl alcohol as a hydrogendonor. It was foundthat the preferredcatalyst was 50 weight% zinc oxide-magnesiumoxide catalyst prepared by calcininga mixtureof zincnitrate and magnesiumoxide at 500°C. The optimumconditions were found to be as follows;reaction tem- perature,near 200°C,total feed rate, 45 moles/1.of catalyst/hr.,feed ratio of isopropylalcohol per acrolein,10 moles. Under theseconditions, the yieldsof allyl alcoholof 80-65% at 80-90% conversion of acroleinwere obtained. INTRODUCTION Acrolein has two reactive functional groups, one is carbonyl group and the other is carbon-carbon double bond. Selective reduction of acrolein to allyl alcohol has been studied by several investigators. The reaction was generally carried out by the following two methods: (1) the Meerwein-Ponndorf-Verley reduction1-3), (2) vapor phase hydrogen transfer reaction with various metal oxide catalysts using an alcohol as a hydrogen donor4-11> The liquid phase reaction has some technical difficulties owing to the polymeri- zation of acrolein especially at high conversion. Therefore, in the present work, the more promising vapor phase reaction has been studied to find an effective catalyst and favorable reaction conditions.
  • Conversion of Glycerol Into Allyl Alcohol Over Potassium-Supported Zirconia-Iron Oxide Catalyst

    Conversion of Glycerol Into Allyl Alcohol Over Potassium-Supported Zirconia-Iron Oxide Catalyst

    Title Conversion of glycerol into allyl alcohol over potassium-supported zirconia-iron oxide catalyst Author(s) Konaka, Aya; Tago, Teruoki; Yoshikawa, Takuya; Nakamura, Ayaka; Masuda, Takao Applied catalysis b-environmental, 146, 267-273 Citation https://doi.org/10.1016/j.apcatb.2013.03.007 Issue Date 2014-03 Doc URL http://hdl.handle.net/2115/54715 Type article (author version) File Information Manuscript_Glycerol to Allyl Alcohol .pdf Instructions for use Hokkaido University Collection of Scholarly and Academic Papers : HUSCAP Conversion of Glycerol into Allyl Alcohol over Potassium-Supported Zirconia-Iron Oxide Catalyst Aya Konaka, Teruoki Tago*, Takuya Yoshikawa, Ayaka Nakamura, and Takao Masuda Research Group of Chemical Engineering, Division of Chemical Process Engineering, Faculty of Engineering, Hokkaido University, N13W8, Kita-ku, Sapporo, Hokkaido, Japan 060-8628 * Corresponding author should be addressed E-mail: [email protected] Tel: +81-11-706-6551 Fax: +81-11-706-6552 1 Abstract The catalytic conversion of glycerol was performed with iron oxide-based catalysts for production of allyl alcohol using a fixed-bed flow reactor at 623 K under atmospheric pressure. The glycerol dehydration proceeds on acid sites of catalysts while the allyl alcohol production is assumed to be catalyzed by non-acidic sites of catalysts through a hydrogen transfer mechanism. Different alkali metals, including Na, K, Rb, and Cs were supported on ZrO2-FeOX and all of them gave impressively higher allyl alcohol yield and suppressed glycerol dehydration due to the reduced catalyst acidic property. K-supported ZrO2-FeOX (K/ZrO2-FeOX) was chosen for further studies, and allyl alcohol yield remarkably increased up to 27 mol%-C at the K content of 3-5 mol%.
  • Silfort* SHC1200 Silfort* SHC1200

    Silfort* SHC1200 Silfort* SHC1200

    Technical Data Sheet SilFORT* SHC1200 SilFORT* SHC1200 Description SilFORT SHC1200 Hard Coat SHC1200 hard coat has been found to yield a clear mar-resistant film when applied to a suitably prepared plastic substrate. It can be applied by flow, dip or spray coating. SilFORT SHP401 Primer SHP401 air-dried primer is used as an adhesion promoter for SHC1200 hard coat on polycarbonate resin. It can be applied by flow, dip or spray coating. Key Features and Benefits Fast cure Abrasion resistance Scratch resistance Good clarity Solvent/chemical resistance SHP401 Primer No thermal cure required Improves coating adhesion Improves water resistance Page 1 of 6 *SilFORT ist ein Markenname der Momentive Performance Materials Inc. SilFORT* SHC1200 Improves ultraviolet resistance SHP401 Primer/SHC1200 Hard Coat on polycarbonate (2 - 4 micron Topcoat Thickness) Cured Film Properties Film Thickness, slow dip coat, 10-18 cm/min 2 – 4 micron withdrawal,18-20% solids at 22C Taber Abrasion, 500 cycles 500G on primed < 6.0 % Haze measured per polycarbonate (CS10F wheel) ASTM D1003. * Index of Refraction 1.4 *Humidity during coating and testing will affect final values. Typical Physical Properties Property SHC1200 Hard Coat SHP401 Primer Solids Content, % 20 ± 1 2.1 ± 0.2 Methanol, Isobutanol, 1-Methoxy-2-propanol, Diacetone Solvent Isopropanol Alcohol Flash Point, PMCC 19.4C 36.1C Density, g/cm3 0.911 0.959 pH 7.3 ± 0.2 - Viscosity, cstk @ 25°C 20 ± 3 4 - 7 Dry Film Thickness, 2.75 - 4.5 0.5 micron VOC, g/l 710 937 Patent Status Nothing contained herein shall be construed to imply the nonexistence of any relevant patents or to constitute the permission, inducement or recommendation to practice any invention covered by any patent, without authority from the owner of the patent.
  • Methanol and Acetone Is in Organic Synthesis

    Methanol and Acetone Is in Organic Synthesis

    Honeywell Burdick & Jackson® Characterization and Evaluation of Technical Grade Solvents and Comparison to their Purified Counterparts S. Lorenz, M. Bosma, A. Kemperman, V. Mohan and J. Przybytek Abstract: Technical grade solvents and their purified counterparts are separately useful for many different applications. One important application for the common solvents acetonitrile, methanol and acetone is in organic synthesis. Another important application for acetonitrile and methanol is as a diluent or mobile phase in chemical analysis, ie: UV-VIS spectroscopy, HPLC and LC-MS. We have observed and identified a number of impurities in these solvents that may interfere with synthesis and/or accurate analytical testing. For instance, a common contaminant in acetonitrile is acrylonitrile. Trace aldehydes and ketones can be found in methanol. Diacetone alcohol is commonly found in acetone. We have characterized impurity levels in commonly used solvents and will show the variability present in technical grade and purified solvents, using GC, GC-MS and LC-MS. Results on the impurities and their probable effect on synthesis and analytical testing will be presented. METHANOL HPLC Comparison of Methanol Grades HPLC Trace using HPLC Trace using HPLC Method Technical Grade Methanol Purified Methanol 0.200 0.200 Time % % 0.190 0.190 0.180 0.180 (min) Water Methanol 0.170 0.170 0.160 0.160 0.150 0.150 0 95 5 0.140 AU) 0.140 AU) ( ( 0.130 0.130 e e 20 0 100 c 0.120 c 0.120 n 0.110 n 0.110 a a b 0.100 b 0.100 r r 25 0 100 o 0.090 o 0.090 s s 0.080 0.080
  • Alcoholsalcohols

    Alcoholsalcohols

    AlcoholsAlcohols Chapter 10 1 Structure of Alcohols • The functional group of an alcohol is H an -OH group bonded to an sp3 O 108.9° hybridized carbon. C H – Bond angles about the hydroxyl oxygen H H atom are approximately 109.5°. • Oxygen is sp3 hybridized. –Two sp3 hybrid orbitals form sigma bonds to a carbon and a hydrogen. – The remaining two sp3 hybrid orbitals each contain an unshared pair of electrons. 2 Nomenclature of Alcohols • IUPAC names – The parent chain is the longest chain that contains the OH group. – Number the parent chain to give the OH group the lowest possible number. – Change the suffix -etoe -ol.ol • Common names – Name the alkyl group bonded to oxygen followed by the word alcohol.alcohol 3 Nomenclature of Alcohols OH o o 1o OH 1 2 OH 1-Propanol 2-Propan ol 1-Bu tanol (Pro py l alco ho l) (Isoprop yl alcoh ol) (Bu tyl alcoh ol) OH 2o OH 1o OH 3o 2-Butanol 2-M eth yl-1-p ropan ol 2-M eth yl-2-p ropan ol (sec-Butyl alcohol) (Isobutyl alcohol) (tert -Butyl alcohol) 4 Nomenclature of Alcohols • Compounds containing more than one OH group are named diols, triols, etc. CH2 CH2 CH3 CHCH2 CH2 CHCH2 OH OH HO OH HO HO OH 1,2-Ethanediol 1,2-Propanediol 1,2,3-Propanetriol (Ethylene glycol) (Propylene glycol) (Glycerol, Glycerine) 5 Physical Properties • Alcohols are polar compounds. – They interact with themselves and with other polar compounds by dipole-dipole interactions. • Dipole-dipole interaction: The attraction between the positive end of one dipole and the negative end of another.
  • Chemicals That Form Explosive Levels of Peroxides Without Concentration (Safe Storage Time After Opening - 3 Months) Chemical CAS # Synonym State Ref

    Chemicals That Form Explosive Levels of Peroxides Without Concentration (Safe Storage Time After Opening - 3 Months) Chemical CAS # Synonym State Ref

    Group A- Chemicals that form explosive levels of peroxides without concentration (Safe storage time after opening - 3 months) Chemical CAS # Synonym State Ref. 000106- Butadiene(1,3) 1,3-Butadiene gas 4 99-0 000126- 2-Chloro-1,3- Chloroprene (1,3) liquid 4 99-8 butadiene 000821- Divinyl acetylene 1,5-Hexadien- 3-yne liquid 5 08-9 000108- Isopropyl ether liquid 5 20-3 000116- Tetrafluoroethylene gas 4 14-3 000109- Vinyl ether Divinyl ether liquid 5 93-3 000075- 1,1- Vinylidene chloride liquid 5 35-4 Dichloroethylene Group B-Chemicals that form explosive levels of peroxides on concentration (Safe storage time after opening - 12 months) Chemical CAS # Synonym State Ref. 000105- Acetal liquid 5 57-7 000075- Acetaldehyde liquid 4 07-0 000100- Benzyl alcohol liquid 4 51-6 000078- 2-Butanol liquid 4 92-2 000108- Cyclohexanol liquid 4 93-0 000110- Cyclohexene liquid 5 83-8 000822- 2-Cyclohexen-1-ol liquid 4 67-3 000142- Cyclopentene liquid 5 29-0 000091- Decahydronaphthalene liquid 4 17-8 000460- Diacetylene gas 5 12-8 000077- Dicyclopentadiene liquid 5 73-6 Diethylene glycol 000111- Diglyme liquid 5 dimethyl ether 96-6 000123- Dioxane 1,4-Dioxane liquid 5 91-1 Ethylene glycol 000110- Glyme liquid 5 dimethyl ether 71-4 000060- Ethyl ether Diethyl ether liquid 5 29-7 000110- Furan liquid 5 00-9 000589- 4-Heptanol liquid 4 55-9 000626- 2-Hexanol liquid 4 93-7 000098- Isopropyl benzene Cumene liquid 5 82-8 000074- Methyl acetylene Propyne gas 5 99-7 000123- 3-Methyl-1-butanol Isoamyl alcohol liquid 4 51-3 000096- Methyl cyclopentane liquid 5 37-7
  • Synthesis of Higher Alcohols During Alcoholic Fermentation of Rye Mashes

    Synthesis of Higher Alcohols During Alcoholic Fermentation of Rye Mashes

    SCIENTIFIC BULLETIN OF THE TECHNICAL UNIVERSITY OF LODZ No. 1081 Food Chemistry and Biotechnology, Vol. 74 2010 MARTA PIETRUSZKA KATARZYNA PIELECH-PRZYBYLSKA JÓZEF STANISŁAW SZOPA Institute of Fermentation Technology and Microbiology Technical University of Lodz SYNTHESIS OF HIGHER ALCOHOLS DURING ALCOHOLIC FERMENTATION OF RYE MASHES Review: Edyta Kordialik-Bogacka Ph.D. Formation of by-products during alcoholic fermentation is a complex process. Particular attention should be paid to generation of higher alcohols because of its complex mechanism and dynamics. In XIX century the higher alcohols were thought about as “bacterial metabolites of spoilage” that contaminate alcoholic beverages. At the beginning of XX century Ehrlich proved that these compounds were produced by yeast from amino acids and they naturally occurred in all alcoholic beverages derived from spirits of agricultural origin. The quantity and profile of fusel alcohols in the wash depend on many factors such as raw materials used to prepare the sweet mash, yeast strain and the inoculum dose, supplements added to the mash. Investigations of many researchers prove that higher alcohols are formed through catabolic and anabolic pathways. They are either products of amino acid catabolism – as was found by Ehrlich or by-products of amino acid synthesis from pyruvate through the anabolic pathway. The occurrence of fusel alcohols in raw spirits from agricultural distilleries is a result of the presence of amino acids, sugars and products of their metabolism mainly aldehydes, in fermented mashes. Introduction One of Polish Standards regulates allowable concentrations of alcoholic fermentation by-products like methanol, aldehydes, esters and organic acids in raw spirits from agricultural distilleries but it does not refer to higher alcohols [1].